Reference of 87-48-9, 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 87-48-9 as follows.
In a 5L four-necked flask, add 5-bromoisatin 250.0g,1000ml absolute ethanol, stirring, and then slowly add hydrationHydrazine (80%) 81.4g, heated to reflux (80 C)Reaction 2h,Sampling HPLC test, no raw material remaining, the reaction liquid coolingTo about 15 , crystallization 15min, filtered, the filter cake was washed with a small amount of cold ethanol or mother liquor,Then at 50 oven drying 12h, get hydrazone crude. In a 5L four-necked flask, put the crude hydrazide obtained above,Ethylene glycol 1000ml, stirring, adding sodium hydroxide 32.5g,Heated to reflux,Reflux temperature gradually increased from 95 to 115 , the reaction 7h,Sample HPLC test, no raw material remaining, stop heating, cooling to below 30 , the reaction solution was transferred to a 10L bottle, add water 1500ml, with concentrated hydrochloric acid to adjust PH = 2.5 or so, adding methylene chloride 1500ml, The floc was precipitated, filtered, and the layers were separated. The aqueous layer was further extracted with 500 ml of dichloromethane, and the organic layers were combined.The solvent was distilled off under reduced pressure to give 402.4 g of bromoindolinone (Formula II).
According to the analysis of related databases, 87-48-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Ningbo Jiu Sheng Chuangxin Pharmaceutical Technology Co., Ltd.; Li Changlong; Yu Lihuang; He Guojin; Tao Weijian; (7 pag.)CN104693019; (2017); B;,
Indoline – Wikipedia,
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