反応 #5979

反応方程式

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

溶媒

sodium hydroxide

methanol

反応条件

後処理

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued at 60° C. overnight
3. 3
   その他The methanol is removed in vacuum
4. 4
   workup.ADDITIONdiluted with water
5. 5
   ろ過filtered
6. 6
   ろ過filtered
7. 7
   抽出extracted with ethyl acetate
8. 8
   洗浄washed with water
9. 9
   乾燥dried over magnesium sulfate
10. 10
    その他evaporated to dryness

実験手順

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.

出典