Tag: M.W=200-300

Reference of 959235-95-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 959235-95-1 name is 6-(Trifluoromethoxy)indoline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To a solution of 2-(2-(2-((tert-butyldimethylsilyl)oxy)ethoxy)-4-chlorophenyl)-2-((3-methoxy-5-(methylsulfonyl)phenyl)amino)acetic acid 5d (1 .07 g, 1 .97 mmol) inDMF (10 mL) were added HATU (1 .12 g, 2.95 mmol), diisopropylethylamine (976 pL, 5.91 mmol) and 6-(trifluoromethoxy)indoline [CAS 959235-95-1] (400 mg, 1 .97 mmol). The reaction mixture was stirred at room temperature for 2 h. The reaction mixture was diluted with water. The precipitate was filtered off, washed with waterand taken up with EtOAc. The organic layer was washed with a 10% solution ofK2003, water, dried over MgSO4, filtered and the solvent was concentrated under reduced pressure to give 2-(2-(2-((tert-butyldimethylsilyl)oxy)ethoxy)-4-chlorophenyl)-2-((3-methoxy-5-(methylsulfonyl)phenyl)amino)-1 -(6-(trifluoromethoxy)indolin-1-yl)ethanone 6a (1.36 g). The crude compound wasused without purification in the next reaction step.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 6-(Trifluoromethoxy)indoline, and friends who are interested can also refer to it.

Electric Literature of 161596-47-0, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 161596-47-0 as follows.

[0048] (S)-2-(oxiran-2-ylmethyl)isoindoline-1,3-dione (3.87 g, 19.06 mmol, 1.1 eq.) and 4-(4-isocyanatophenyl)morpholin-3-one (3.77 g, 17.29 mmol) were dissolved in chlorobenzene (70 mL) respectively, then heated to 115 C. and lithium iodide (0.23 g, 1.72 mmol) was added. The mixture was reacted for 4 h, white solid was obtained by filtration (6.85 g, yield: 94.09%). [0049] ESI-MS (m/z): 422 (M+H), 444 (M+Na); [0050] 1HNMR (400 MHz, CDCl3) delta: 3.74 (m, 2H), 3.94 (m, 4H), 4.10 (m, 2H), 4.32 (s, 2H), 4.98 (m, 1H), 7.34 (d, 2H), 7.56 (d, 2H), 7.75 (m, 2H), 7.88 (m, 2H); [0051] HPLC: 98.91%.

According to the analysis of related databases, 161596-47-0, the application of this compound in the production field has become more and more popular.

Application of 1677-47-0,Some common heterocyclic compound, 1677-47-0, name is 4,5-Dichloroisatin, molecular formula is C8H3Cl2NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

5,6-Dichloroanthranilic Acid This material was obtained from 4,5-dichloroisatin in 91% yield by the method of B. R. Baker, et al., J. Org. Chem., 17, 141 (1952).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4,5-Dichloroisatin, its application will become more common.

Related Products of 304876-29-7, A common heterocyclic compound, 304876-29-7, name is 2′,3′,5′,6′-Tetrahydrospiro[indoline-3,4′-pyran]-2-one, molecular formula is C12H13NO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Sodium hydride (8.00 mg of a 60% dispersion in mineral oil, 0.207 mmol) was added to a solution of 2′,3′,5′,6I-tetrahydrospiro[indole-3,4′-pyran]-2(lH)-one from Step A (35.0 mg, 0.172 mmol) in DMF (1 mL) at 0 0C. After 1 hr, tert-butyl bromoacetate (0.280 mL, 0.189 mmol) was added and the reaction warmed to ambient temperature. After 18 h, the reaction was partitioned between CH2Cl2 (10 mL) and saturated NH4CI (10 mL). The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to give the title compound. MS: m/z = 318 (M + 1).

The synthetic route of 304876-29-7 has been constantly updated, and we look forward to future research findings.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1677-47-0, name is 4,5-Dichloroisatin, A new synthetic method of this compound is introduced below., name: 4,5-Dichloroisatin

A 10 mL tetrahydrofuran solution of 3.02 g of 2-bromo-1-methoxy-4-methylbenzene was added dropwise under a nitrogen atmosphere to a suspension of 360 mg of magnesium in 10 mL of tetrahydrofuran, after which the reaction mixture was stirred for 30 minutes under heating and reflux, and then allowed to stand and cool to room temperature. 1.50 g of 4,5-dichloro-1H-indol-2,3-dione was added under ice cooling and a nitrogen atmosphere to a 40 mL tetrahydrofuran solution of 310 mg of sodium hydride, and the reaction mixture was stirred for 1 hour. After this, 20 mL of a previously prepared tetrahydrofuran solution of bromo(2-methoxy-5-methylphenyl)magnesium was added dropwise over a period of 20 minutes, and the reaction mixture was stirred for 4.5 hours at the same temperature, after which 50 mL of a saturated ammonium chloride aqueous solution was added, and the reaction mixture was stirred for 30 minutes at room temperature. After liquid separation, the aqueous layer was extracted with ethyl acetate (30 mL × 3), the combined organic layer was washed with saturated brine and dried with sodium sulfate, and the drying agent was then filtered off and the solvent was distilled off under reduced pressure. The residue thus obtained was stirred and washed with isopropyl ether and the solids were filtered off to obtain 1.23 g of the titled compound (yellow solid). MS (ESI pos.) m/z : 360([M+Na]+), (ESI neg.) m/z : 336([M-H]-) 1 H-NMR (200 MHz, DMSO-d6) delta (ppm); 2.31 (s, 3 H), 3.38 (s, 3 H), 6.64 – 6.87 (m, 3 H), 7.00-7.13 (m, 1 H), 7.42 (d, J=8.4 Hz, 1 H), 7.68 (d, J=2.2 Hz, 1 H), 10.61 (s, 1 H)

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 153744-36-6, name is Methyl 3-(1,3-dioxoisoindolin-2-yl)-2-hydroxypropanoate, A new synthetic method of this compound is introduced below., Formula: C12H11NO5

General procedure: tert-Butyl(2-iodoethoxy) diphenylsilane (1.4 eq) andAg2CO3 (4.0 eq) were added to a suspension of the aminoacid derivative (1.0 eq) in toluene (10.0 ml). The reactionmixture was stirred in a pressure tube at 120 C until TLCindicated complete consumption of the amino acid derivative,cooled to rt, filtered through a paper filter and reducedin vacuum. The residue was purified by flash columnchromatography on silica (eluent: pentane/Et2O 7:3).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 84764-41-0, name is 2-(2-(2-Methyl-1,3-dioxolan-2-yl)ethyl)isoindoline-1,3-dione, A new synthetic method of this compound is introduced below., HPLC of Formula: C14H15NO4

20 g of 2- (2- (2-methyl-1,3-dioxolan-2-yl) ethyl) isoindoline-1,3-dione was dissolved in 200 ml Liter of methanol, and to the inside of a 4.60 grams of 98% purity of hydrazine hydrate. The reaction was stirred for 12 hours under reflux. reaction After the end of the reaction, the reaction system was allowed to stand at room temperature and suction filtered. The filtrate was dried under reduced pressure to give crude 2- (2-methyl-1,3-Dioxolan-2-yl) ethylamine was used directly in the next step in a yield of 99%.

The synthetic route of 84764-41-0 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 161596-47-0, name is (S)-2-(Oxiran-2-ylmethyl)isoindoline-1,3-dione, belongs to indolines-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 161596-47-0, Recommanded Product: 161596-47-0

((S)-2-(oxiran-2-ylmethyl)isoindoline-1,3-dione (4.56g, 22.46mmol, 1.3eq.) and 4-(4-isocyanatophenyl)morpholin-3-one (3.77g, 17.29mmol) were dissolved in isoamyl acetate (70mL) respectively, and heated to 120C. Then magnesium chloride (0.12g, 1.28mmol) was added, the mixture was reacted for 4h, white solid was obtained by filtration (6.97g, yield:95.5%). ESI-MS(m/z): 422(M+H), 444(M+Na); 1HNMR(400MHz, CDCl3) delta: 3.74(m, 2H), 3.94(m, 4H), 4.10(m, 2H), 4.32(s, 2H), 4.98(m, 1H), 7.34(d, 2H), 7.56(d, 2H), 7.75(m, 2H), 7.88(m, 2H); HPLC: 98.82%

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, (S)-2-(Oxiran-2-ylmethyl)isoindoline-1,3-dione, other downstream synthetic routes, hurry up and to see.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 106352-01-6, name is 3-((1,3-Dioxoisoindolin-2-yl)methyl)benzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-((1,3-Dioxoisoindolin-2-yl)methyl)benzoic acid

To 3-(1 ,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-benzoic acid (300 mg, 1.066 mmol) in DCM (1 mL9 are added at O0C triethylamine (164 uL, 1.173 mmol) and ethylchloroformate (112 uL, 1.173 mmol). After stirring at O0C during 15 min and filtration, the obtained solution is added at 0C to NaBH4 (61 mg, 1.599 mmol) in water (400 uL) before stirring at 00C during 30 min and at rt during 2h. The solution is acidified to pH 3 with an aqueous 1N HCI solution, extracted with ethylacetate, the organic phase is dried and evaporated to give a crude compound before purification by flash chromatography on silica gel (eluent: cyclohexane/ethyl acetate 9/1 to 1/1) to yield a colorless gum. TLC, Rf (cyclohexane/ethyl acetate 1/1) = 0.15.

The synthetic route of 106352-01-6 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 18711-13-2,Some common heterocyclic compound, 18711-13-2, name is 4,7-Dichloroindoline-2,3-dione, molecular formula is C8H3Cl2NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

4,7-Dichloroisotin (4.26 g, 19.7 mmol, 1 equiv, Alfa Aesar lot 10173559) and MeOH (70 mL, 16.4 vol) were charged to a 250-mL, three-neck, round-bottom flask equipped with nitrogen line, overhead mechanical stirrer, and a temperature probe. Diethylamine (0.43 g, 0.30 equiv, Sigma- Aldrich lot SHBD5313V) was added over 1 min via syringe (the slurry becomes dark red). l-[4-(Methylamino)phenyl]ethanone 3 (11.4 g, 3.9 equiv, Sigma- Aldrich lot 01129HHV) was added in portions via a plastic funnel, over 15 min. The funnel was rinsed with MeOH (2 x 15 mL, 7.0 vol). The reaction was stirred at ambient temperature (approximately 18-20 C) and periodically sampled for in-process control (IPC) by HPLC. After 40 h of reaction, additional diethylamine was charged to the reaction via syringe (0.16 g, 0.11 equiv) and the stirring continued at ambient temperature. After 64 h, a light slurry formed. Additional diethylamine was charged to the reaction via syringe (0.13 g, 0.09 equiv) and the stirring continued at ambient temperature. After 92 h of reaction IPC by HPLC analysis showed 2.1% AUC of isatin 1 present in the reaction mixture. Additional diethylamine was charged to the reaction via syringe (0.07 g, 0.05 equiv) for a total of 0.55 equiv of base and the stirring continued at ambient temperature over the weekend. After a total of seven days, the reaction was concentrated under reduced pressure (water bath <40 C), the solid residue was dissolved in a mixture of dichloromethane (450 mL) and MeOH (50 mL) at 30 C, and adsorbed over 20 g of silica gel. Purification was carried out in a Combiflash CompanionTM XL system with a RediSep disposable flash 220 g silica gel column (catalog 69-2203-422). Elution of the residual starting material 3 was accomplished with dichloromethane (approximately 20 column vol, while the product TK- 202 was eluted with 10% methanol in dichloromethane. The product containing fractions, where product had already started to precipitate, were combined in two different lots and partially concentrated under reduced pressure. The resulting slurries were filtered and the solid cakes were washed with MeOH to afford two fractions that were dried under high vacuum at ambient temperature for 24 h, then 50 C for 24 h, to afford lot BIO-W-30-17 and lot BIO-W-30-18. The filtrate from both crystallizations were combined and subjected to a second chromatographic purification (on a 40-g RediSep Gold column, catalog 69- 2203-347) using a gradient from dichloromethane to 5% methanol in dichloromethane for elution. The product containing fractions (purity higher than 99% AUC by HPLC) were combined and the product was allowed to precipitate over 2 h. The solid was filtered off, washed with methanol, and dried under high vacuum for 24 h at 50 C to afford lot BIOW- 30-19. A second set of fractions containing product of approximately 95% AUC purity by HPLC were combined, the solid was filtered off, re-dissolved in dichloromethane, and added 20% methanol to precipitate overnight. The precipitated TK-202 was filtered and washed with methanol, then dried under high vacuum for 24 h at 50 C to afford lot BIO-W-30-16. The total combined weight of 5.99 g corresponds to 83% yield of compound. Solid is off- white (with a very pale peach to tan shade). These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4,7-Dichloroindoline-2,3-dione, its application will become more common.