反应详情

1.54 g (10 mmol) of 4-mercaptobenzoic acid and 40 ml of pyridine were introduced into a round-bottomed flask. A solution of 3.75 g (10 mmol) of 3-(1-adamantyl)-4-methoxyethoxymethoxybenzoyl chloride prepared in Example 10(c) was added dropwise and the mixture was stirred at room temperature for six hours. The mixture was evaporated to dryness, the residue was taken up in water and ethyl ether. The organic phase was separated out after settling had taken place, washed with water, dried over magnesium sulfate and evaporated. The solid obtained was recrystallized from a diisopropyl ether/methanol mixture, filtered off and dried. 2.94 g (59%) of 4-[3-(1-adamantyl)-4-methoxyethoxymethoxybenzoylthio]benzoic acid, having a melting point of 187°-8° C., were recovered.

1. customThe mixture was evaporated to dryness
2. customThe organic phase was separated out
3. washwashed with water
4. dry with materialdried over magnesium sulfate
5. customevaporated
6. customThe solid obtained
7. customwas recrystallized from a diisopropyl ether/methanol mixture
8. filtrationfiltered off
9. customdried
10. customwere recovered