反应详情

A suspension of thioxanthen-9-one [31] (2 g, 9.42 mmol) in anhydrous CH3OH (30 mL) was stirred under N2 and NaBH4 (1.42 g, 37.68 mmol) was added slowly in portions over 15 min. After complete addition the reaction mixture was heated at reflux (3 hr.) and cooled to room temperature. Ice-water was added and the reaction mixture was extracted with CH2Cl2 (3×50 mL). The combined CH2Cl2 extracts were washed with water, brine, dried (MgSO4). The solvent was removed under reduced pressure to give a yellow solid, which was recrystallized from pet.ether to give 1.87 g (93%) of the alcohol as pale yellow needles, mp 104-105° C.

1. additionAfter complete addition the reaction mixture
2. temperaturewas heated
3. temperatureat reflux (3 hr.)
4. extractionthe reaction mixture was extracted with CH2Cl2 (3×50 mL)
5. washThe combined CH2Cl2 extracts were washed with water, brine
6. dry with materialdried (MgSO4)
7. customThe solvent was removed under reduced pressure
8. customto give a yellow solid, which
9. customwas recrystallized from pet