반응 #44676

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4-(2-fluoro-4-nitrophenoxy)-1,2-benzisoxazole-3-amine

4-(2-Fluoro-4-nitrophenoxy)-1,2-benzisoxazole-3-amine

tin(II) chloride dihydrate

sodium bicarbonate

→

4-(4-Amino-2-fluorophenoxy)-1,2-benzisoxazole-3-amine

용매

ethyl acetate

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후처리

1. 1
   온도After cooling to room temperature
2. 2
   기타gives a colorless precipitate
3. 3
   workup.ADDITION5 g of kieselguhr are added to the suspension
4. 4
   여과the mixture is filtered
5. 5
   추출The filtrate is extracted repeatedly with ethyl acetate
6. 6
   세척The combined organic phases are washed with water
7. 7
   건조dried over sodium sulfate
8. 8
   기타Removal of the solvent under reduced pressure
9. 9
   기타gives the product

실험 절차

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.

출처