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Trimethylsilyl triflate → (3S,4R)-4-[2-(1-allyloxycarbonylpyrrolidin-3-yl)-2-oxoethyl]-3-[(1R)-1-t-butyldimethylsilyloxyethyl]-2-oxoazetidine

HRID 1029607
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HRID 1029607 반응식
C(O[C@H:5]1[NH:8][C:7](=[O:9])[C@@H:6]1[C@H:10]([O:12][Si:13]([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14])[CH3:11])(=O)C.FC(F)(F)S(O[Si](C)(C)C)(=O)=O.[C:32]([CH:35]1[CH2:39][N:38]([C:40]([O:42][CH2:43][CH:44]=[CH2:45])=[O:41])[CH2:37][CH2:36]1)(=[O:34])[CH3:33].C(=O)([O-])O.[Na+]>ClCCl.O.C(OCC)(=O)C.C(N(CC)CC)C>[CH2:43]([O:42][C:40]([N:38]1[CH2:37][CH2:36][CH:35]([C:32](=[O:34])[CH2:33][C@H:5]2[NH:8][C:7](=[O:9])[C@@H:6]2[C@H:10]([O:12][Si:13]([C:16]([CH3:17])([CH3:18])[CH3:19])([CH3:14])[CH3:15])[CH3:11])[CH2:39]1)=[O:41])[CH:44]=[CH2:45]
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참가 물질

9

반응물 4

HCID 65367Trimethylsilyl triflate2회HCID 516892Sodium BicarbonateHCID 10935078AzetidonHCID 151171953-Acetyl-1-allyloxycarbonylpyrrolidine

생성물 1

HCID 15117203(3S,4R)-4-[2-(1-allyloxycarbonylpyrrolidin-3-yl)-2-oxoethyl]-3-[(1R)-1-t-butyldimethylsilyloxyethyl]-2-oxoazetidine수율 55.7%

시약·촉매·용매

4
HCID 962Water용매HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매2회HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a solution of (3R,4R)-4-acetoxy-3-[(1R)-1-t-butyldimethylsilyloxyethyl]-2-oxoazetidine (2.2 g) and triethylamine (1.1 ml) in dichloromethane (20 ml) was added trimethylsilyl trifluoromethanesulfonate (1.5 ml) at -60° C. under nitrogen, and the mixture was stirred at 0° C. for 30 minutes (Solution A). To a solution of 4-acetyl-1-allyloxycarbonylpyrrolidine (1.0 g) and triethylamine (0.71 ml) in dichloromethane (10 ml) was added trimethylsilyl trifluoromethanesulfonate (0.98 ml) at -60° C. under nitrogen and the resulting mixture was stirred at 0° C. for 30 minutes. To this mixture was added dropwise the Solution A at 0° C. under nitrogen, and the mixture was stirred for additional 4 hours at 0° C. The reaction mixture was taken up into a mixture of ethyl acetate and water and the mixture was stirred at ambient temperature for 2 hours. After adjusting pH to around 6.5 with aqueous sodium hydrogen carbonate, the organic layer was separated, washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel eluting with a mixture of n-hexane and ethyl acetate (1:2, V/V) to give (3S,4R)-4-[2-(1-allyloxycarbonylpyrrolidin-3-yl)-2-oxoethyl]-3-[(1R)-1-t-butyldimethylsilyloxyethyl]-2-oxoazetidine (1.2 g).

후처리

  1. stirringthe mixture was stirred for additional 4 hours at 0° C
  2. stirringthe mixture was stirred at ambient temperature for 2 hours
  3. customthe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was chromatographed on silica gel eluting with a mixture of n-hexane and ethyl acetate (1:2, V/V)

출처 및 근거

ORD 기록
ord-d0596760c065400d8034f3db503bac08
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05102877

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