反応 #2267079

反応方程式

14

6-Acetylamino-3-methyl-1-(4-nitrophenyl)-7-methoxyisochroman

sodium hydroxide

HCl

→

22

6-Acetylamino-1-hydroxy-3-methyl-1-(4-nitrophenyl)-7-methoxyisochroman

溶媒

DMSO

DMF

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate three times
2. 2
   洗浄The combined organic phase was washed with water
3. 3
   乾燥dried over Na2SO4
4. 4
   その他Removal of the solvent

実験手順

A solution of 14 (1.8 g) in 5 ml of DMSO and 30 ml of DMF was cooled to 8-12° C. and air was passed through the mixture. To the solution was added 1.2 ml of 50% aqueous sodium hydroxide in one portion and the resulting mixture was stirred for 5 hours. HCl (1 N) was added, and extracted with ethyl acetate three times. The combined organic phase was washed with water, dried over Na2SO4. Removal of the solvent afforded 22 (1.9 g) as a syrup, which was used directly for the next step.

出典