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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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N-Ethylpiperidine → (3S,4R)-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]-4-[(1R)-1,3-dimethyl-3-(trimethylsilyloxy)-2-oxobutyl]-2-azetidinone

HRID 1461485
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HRID 1461485 반응식
C(N1CCCCC1)C.[CH3:9][C:10]([O:16][Si:17]([CH3:20])([CH3:19])[CH3:18])([C:12](=[O:15])[CH2:13][CH3:14])[CH3:11].C(O[C@H:25]1[NH:28][C:27](=[O:29])[C@@H:26]1[C@H:30]([O:32][Si:33]([C:36]([CH3:39])([CH3:38])[CH3:37])([CH3:35])[CH3:34])[CH3:31])(=O)C>ClCCl>[Si:33]([O:32][C@@H:30]([C@@H:26]1[C@@H:25]([C@@H:13]([CH3:14])[C:12](=[O:15])[C:10]([CH3:9])([O:16][Si:17]([CH3:18])([CH3:20])[CH3:19])[CH3:11])[NH:28][C:27]1=[O:29])[CH3:31])([C:36]([CH3:37])([CH3:38])[CH3:39])([CH3:34])[CH3:35]
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참가 물질

5

반응물 3

HCID 13007N-EthylpiperidineHCID 10935078AzetidonHCID 126414662-Methyl-2-(trimethylsilyloxy)-3-pentanone

생성물 1

HCID 57183497(3S,4R)-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]-4-[(1R)-1,3-dimethyl-3-(trimethylsilyloxy)-2-oxobutyl]-2-azetidinone수율 36.6%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매
3회

실험 절차

To a suspension of stannous trifluoromethanesulfonate (2.18 g) and N-ethylpiperidine (590 mg) in dichloromethane (15 ml) was added dropwise a solution of 2-methyl-2-(trimethylsilyloxy)-3-pentanone (785 mg) in dichloromethane (2 ml) at -78° C. under argon atmosphere. After stirring for 30 minutes, a solution of (3R,4R)-4-acetoxy-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]-2-azetidinone (300 mg) in dichloromethane (3 ml) was added dropwise to the mixture. The reaction mixture was allowed to warm to room temperature and stirred at the same temperature for 3 hours. The mixture was quenched with phosphate butter (pH 7). The organic layer was filtered with celite, washed with dichloromethane, dried over magnesium sulfate and evaporated. The residue was chromatographed on silica gel (9 g) eluting with a mixture of ethyl acetate and hexane (1:10, V/V) to give (3S,4R)-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]-4-[(1R)-1,3-dimethyl-3-(trimethylsilyloxy)-2-oxobutyl]-2-azetidinone (159 mg).

후처리

  1. stirringstirred at the same temperature for 3 hours
  2. customThe mixture was quenched with phosphate butter (pH 7)
  3. filtrationThe organic layer was filtered with celite
  4. washwashed with dichloromethane
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was chromatographed on silica gel (9 g)
  8. washeluting with a mixture of ethyl acetate and hexane (1:10, V/V)

출처 및 근거

ORD 기록
ord-3018223316cf4dd08f36f5bdc7530aad
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05075437

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