反应 #2267069

反应方程式

3

3-Methyl-1-(4-nitrophenyl)-6-methoxyisochroman

sodium hydroxide

HCl

→

crude product

1-Hydroxy-3-methyl-1-(4-nitrophenyl)-6-methoxyisochroman

溶剂

DMSO

DMF

反应条件

后处理

1. 1
   萃取extracted with ethyl acetate three times
2. 2
   洗涤The combined organic phase was washed with water in order
3. 3
   其他to remove DMF
4. 4
   干燥dried over Na2SO4
5. 5
   其他Removal of the solvent

实验过程

A solution of 3 (1.3 g) in 4 ml of DMSO and 24 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 in order to remove DMF, dried over Na2SO4. Removal of the solvent afforded syrup crude product (1.6 g), which was used directly for the next step.

来源