反应详情

2.26 g (59.8 mmol) of sodium borohydride was added to 7 ml of tetrahydrofuran, and while cooling on ice, 15 ml of tetrahydrofuran solution containing 6.78 g (31.5 mmol) of the compound (137) obtained above was dropped to the solution through 20 minutes. Then, 15 ml of tetrahydrofuran solution containing 10 ml of borontrifluoride-ether complex was dropped to the solution through 10 minutes, and after stirring for 30 minutes as was, the solution was stirred for 1 hour at room temperature. To 130 ml of water containing 9.6 g of sodium hydrogen carbonate and 170 ml of methylene chloride, the reaction solution was added slowly, and the obtained solution was stirred overnight at room temperature. The organic layer was separated, and after drying over magnesium sulfate, the solvent was removed by distillation. To the residue, n-hexane was added to crystallize, and the crystals were filtered off and washed with n-hexane to obtain 5.43 g of the subject compound (138) in a 86% yield.

1. customobtained
2. additionabove was dropped to the solution through 20 minutes
3. additionwas dropped to the solution through 10 minutes
4. stirringthe solution was stirred for 1 hour at room temperature
5. stirringthe obtained solution was stirred overnight at room temperature
6. customThe organic layer was separated
7. dry with materialafter drying over magnesium sulfate
8. customthe solvent was removed by distillation
9. additionTo the residue, n-hexane was added
10. customto crystallize
11. filtrationthe crystals were filtered off
12. washwashed with n-hexane