反应详情

温度

70 °C

120 mg (0.41 mmol) of 4-(2-fluoro-4-nitrophenoxy)-1,2-benzisoxazole-3-amine (from example VI) and 468 mg (2.07 mmol) of tin(II) chloride dihydrate are dissolved in 8 ml of ethyl acetate and heated at 70° C. for 4 hours. After cooling to room temperature, the reaction solution is adjusted to pH 9 using saturated sodium bicarbonate solution, which gives a colorless precipitate. 5 g of kieselguhr are added to the suspension, and the mixture is filtered. The filtrate is extracted repeatedly with ethyl acetate. The combined organic phases are washed with water and dried over sodium sulfate. Removal of the solvent under reduced pressure gives the product.

1. temperatureAfter cooling to room temperature
2. customgives a colorless precipitate
3. addition5 g of kieselguhr are added to the suspension
4. filtrationthe mixture is filtered
5. extractionThe filtrate is extracted repeatedly with ethyl acetate
6. washThe combined organic phases are washed with water
7. dry with materialdried over sodium sulfate
8. customRemoval of the solvent under reduced pressure
9. customgives the product