반응 #5979

반응 방정식

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

용매

sodium hydroxide

methanol

반응 조건

후처리

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued at 60° C. overnight
3. 3
   기타The methanol is removed in vacuum
4. 4
   workup.ADDITIONdiluted with water
5. 5
   여과filtered
6. 6
   여과filtered
7. 7
   추출extracted with ethyl acetate
8. 8
   세척washed with water
9. 9
   건조dried over magnesium sulfate
10. 10
    기타evaporated to dryness

실험 절차

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.

출처