反应详情

To a solution of 300 mg of 5-acetylthio compound prepared in (2) in the mixture of 1.3 ml of methanol and 0.6 ml of tetrahydrofuran was dropped 1.35 ml of 5% aqueous solution of sodium hydroxide and the mixture was stirred for 20 minutes at ambient and then concentrated under reduced pressure. 2 ml of water was added to the residue and the mixture was acidified to pH 1 with 1N hydrochloric acid under cooled with ice. The mixture was extracted with diethyl ether and the extract was washed successively with water and a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to give 210 mg of the title compound as crude product having following physical data.

1. concentrationthen concentrated under reduced pressure
2. addition2 ml of water was added to the residue
3. temperatureunder cooled with ice
4. extractionThe mixture was extracted with diethyl ether
5. washthe extract was washed successively with water
6. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure