반응 #42672

반응 방정식

tert-butyl [(3R,6S)-6-(2,3-difluorophenyl)-2-thioxoazepan-3-yl]carbamate

1-aminobutan-2-ol

→

title compound

수율 108.5%

tert-Butyl {(3R,6S)-6-(2,3-difluorophenyl)-2-[(2-hydroxybutyl)imino]azepan-3-yl}carbamate

수율 108.5%

용매

ethanol

반응 조건

후처리

1. 1
   여과The mixture was filtered
2. 2
   농축concentrated
3. 3
   workup.ADDITIONSaturated aqueous sodium carbonate was added
4. 4
   추출the mixture was extracted with dichloromethane (3×)
5. 5
   건조The combined organic extracts were dried over sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

Mercury(II) chloride (174 mg, 0.640 mmol) was added to a solution of tert-butyl [(3R,6S)-6-(2,3-difluorophenyl)-2-thioxoazepan-3-yl]carbamate (190 mg, 0.533 mmol) and 1-aminobutan-2-ol (152 μL, 1.60 mmol) in ethanol (5 mL) at 55° C. After 30 min, the reaction was allowed to cool to ambient temperature. The mixture was filtered and concentrated. Saturated aqueous sodium carbonate was added and the mixture was extracted with dichloromethane (3×). The combined organic extracts were dried over sodium sulfate, filtered, and concentrated to give the title compound (238 mg). MS 412.2 (M+1).

출처