反应详情

温度

200 °C

A mixture of 24.2 g (82.5 mmol) of 2-({6-methoxy}-1H-indazol-3-yl)-1H-isoindole-1,3(2H)-dione and 73.4 g (0.635 mol) of piridine hydrochloride was heated at 200° C. for 4 hours. The resulting brown solution was cooled to 140° C. and slowly poured in a well stirred mixture of 250 ml of 0.2 N HCl and 350 ml of ethyl acetate. The organic layer was separated and the aqueous layer was salted (45 g of NaCl) and extracted twice with 350 ml of ethyl acetate. Organic extracts were dried over sodium sulfate and concentrated under vacuum to small volume. The precipitate was filtered off and dried: 15.89 g of product as yellow solid were obtained. Yield=68.9%. mp=265-270° C. dec.

1. temperatureThe resulting brown solution was cooled to 140° C.
2. additionslowly poured in a well
3. customThe organic layer was separated
4. extractionextracted twice with 350 ml of ethyl acetate
5. dry with materialOrganic extracts were dried over sodium sulfate
6. concentrationconcentrated under vacuum to small volume
7. filtrationThe precipitate was filtered off
8. customdried