1-Amino-2-butanol → HCID 178459298、化合物

HRID 14394

反応式

HRID 14394 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 178459298HCID 178459298、化合物収率 108.5%

試薬・触媒・溶媒 2

HCID 24085Mercuric Chloride触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f084035ce61e4d8d95185cf8263d086c
出典データセット
uspto-grants-2010_06
特許番号
US07732438B2

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