反应 #5979

反应方程式

sodium

methyl 1-acetylamino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylate

→

1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid

溶剂

sodium hydroxide

methanol

反应条件

后处理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued at 60° C. overnight
3. 3
   其他The methanol is removed in vacuum
4. 4
   workup.ADDITIONdiluted with water
5. 5
   过滤filtered
6. 6
   过滤filtered
7. 7
   萃取extracted with ethyl acetate
8. 8
   洗涤washed with water
9. 9
   干燥dried over magnesium sulfate
10. 10
    其他evaporated to dryness

实验过程

To a solution of 0.3 g of sodium in 15 ml methanol is added 0.6 g of methyl 1-acetylamino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylate. Stirring is continued at 60° C. for two days. This is then diluted with 5 ml 1N sodium hydroxide and stirring continued at 60° C. overnight. The methanol is removed in vacuum, diluted with water, filtered, acidified with acetic acid, filtered, extracted with ethyl acetate, washed with water, dried over magnesium sulfate and evaporated to dryness to obtain 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid. This is purified by crystallization from ethyl acetate/ether.

来源