反応 #44676

反応方程式

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

溶媒

ethyl acetate

反応条件

後処理

1. 1
   温度After cooling to room temperature
2. 2
   その他gives a colorless precipitate
3. 3
   workup.ADDITION5 g of kieselguhr are added to the suspension
4. 4
   ろ過the mixture is filtered
5. 5
   抽出The filtrate is extracted repeatedly with ethyl acetate
6. 6
   洗浄The combined organic phases are washed with water
7. 7
   乾燥dried over sodium sulfate
8. 8
   その他Removal of the solvent under reduced pressure
9. 9
   その他gives the product

実験手順

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.

出典