反应详情

To a 1M of LAH (30 mL) in THF was added 2b (630 mg, 3.88 mmol) in portion. The reaction mixture was stirred at rt for 2 h, then refluxed for 1 h. The reaction mixture was quench with 1 part of H2O (10-mL), one part of 15% NaOH (5 mL) and another part of H2O (5 mL). The aqueous layer was extracted with EtOAc. The EtOAc layer was dried over Na2SO4 and filtered. The solvent was evaporated under reduced pressure to afford 2c (320 mg, 56%) as an oil. MS (ES) m/z 150 [M+H]+.

1. temperaturerefluxed for 1 h
2. customThe reaction mixture was quench with 1 part of H2O (10-mL), one part of 15% NaOH (5 mL)
3. extractionThe aqueous layer was extracted with EtOAc
4. dry with materialThe EtOAc layer was dried over Na2SO4
5. filtrationfiltered
6. customThe solvent was evaporated under reduced pressure