1-Amino-2-butanol → HCID 178459298, 화합물

HRID 14394

반응식

HRID 14394 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:9]1[CH2:15][NH:14][C:13](=S)[C@H:12]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH2:10]1.[NH2:25][CH2:26][CH:27]([OH:30])[CH2:28][CH3:29]>C(O)C.[Hg](Cl)Cl>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:9]1[CH2:15][NH:14][C:13](=[N:25][CH2:26][CH:27]([OH:30])[CH2:28][CH3:29])[C@H:12]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH2:10]1

참가 물질

5

반응물 2

HCID 261071-Amino-2-butanolHCID 59734935tert-Butyl (3R,6S)-6-(2,3-difluorophenyl)-2-thioxoazepan-3-ylcarbamate

생성물 1

HCID 178459298HCID 178459298, 화합물수율 108.5%

시약·촉매·용매 2

HCID 24085Mercuric Chloride촉매HCID 702Ethanol용매

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).

후처리

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. additionSaturated aqueous sodium carbonate was added
  4. extractionthe mixture was extracted with dichloromethane (3×)
  5. dry with materialThe combined organic extracts were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f084035ce61e4d8d95185cf8263d086c
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732438B2

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