HCID 53918863, 화합물 → HCID 53653167, 화합물

HRID 653248노트

반응식

HRID 653248 반응식
[C:1]([O:4][C@@H:5]1[NH:8][C:7](=[O:9])[C@H:6]1[NH:10][C:11]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)(=O)C>CO.C([O-])(=O)C.[Zn+2].C([O-])(=O)C>[CH3:1][O:4][C@H:5]1[NH:8][C:7](=[O:9])[C@H:6]1[NH:10][C:11]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

4

반응물 1

HCID 53918863HCID 53918863, 화합물

생성물 1

HCID 53653167HCID 53653167, 화합물수율 32.8%

시약·촉매·용매 2

HCID 11192Zinc Acetate촉매HCID 887Methanol용매

실험 절차

To a solution of 3 g of (3S,4S)-4-acetoxy-3-tritylamino-2-oxoazetidine in 30 ml of methanol is added 1.7 g of zinc acetate, and the mixture is refluxed for 30 minutes. The reaction mixture is concentrated under reduced pressure, followed by addition of ethyl acetate. The resulting insolubles are removed by filtration, and the filtrate is concentrated under reduced pressure. The residue is purified on a silica-gel column (ethyl acetate:n-hexane=1:1) to give 0.912 g of (3S,4R)-4-methoxy-3-tritylamino-2-oxoazetidine.

후처리

  1. temperaturethe mixture is refluxed for 30 minutes
  2. concentrationThe reaction mixture is concentrated under reduced pressure
  3. additionfollowed by addition of ethyl acetate
  4. customThe resulting insolubles are removed by filtration
  5. concentrationthe filtrate is concentrated under reduced pressure
  6. customThe residue is purified on a silica-gel column (ethyl acetate:n-hexane=1:1)

출처 및 근거

ORD 기록
ord-75556a0155ed444d96e36a4cfc76686b
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04675397

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