HCID 53918863、化合物 → HCID 53653167、化合物

HRID 620990ノート

反応式

HRID 620990 の反応式
[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

参加物

4

反応物 1

HCID 53918863HCID 53918863、化合物

生成物 1

HCID 53653167HCID 53653167、化合物収率 32.8%

試薬・触媒・溶媒 2

HCID 11192Zinc Acetate触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e89e9cd79b1d4e5bb2a5b1f276616eaf
出典データセット
uspto-grants-1989_04
特許番号
US04822790

反応ノート

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