Discovery of 6-Chloro-5-(2-chloroethyl)indolin-2-one

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118289-55-7, 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 118289-55-7 as follows.

9. Preparation of ZPR in sulfolane In a three necked flask was charged: BITP HC1 (5.14g, 20mmol), Na2C03 (2.33g, 22mmol), NaI (3g, 20mmol) and sulfolane (20ml). The mixture was heated at 90oC and than CEI (5.29g, 23mmol) was added with more sulfolane (10ml) ; the reaction mixture was maintained at 90C for 4. 5h. The mixture was cooled to the room temperature and THF was added (150ml) ; the solid was filtrated and washed with THF. From the mother liquors a second crop was obtained by precipitation with water. The yield of the two crops is 70% (purity by HPLC 98.4%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 118289-55-7, and friends who are interested can also refer to it.

Reference:
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2005/40160; (2005); A2;,
Indoline – Wikipedia,
Indoline | C8H9N – PubChem