反应详情

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.

1. stirringstirring
2. waitcontinued at 60° C. overnight
3. customThe methanol is removed in vacuum
4. additiondiluted with water
5. filtrationfiltered
6. filtrationfiltered
7. extractionextracted with ethyl acetate
8. washwashed with water
9. dry with materialdried over magnesium sulfate
10. customevaporated to dryness