Potassium ethanethioate → HCID 54147731、化合物

HRID 621079ノート

反応式

HRID 621079 の反応式
C([O:4][C@@H:5]1[NH:8][C:7](=O)[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.[C:30]([O-:33])(=[S:32])[CH3:31].[K+]>CO.O>[C:30]([S:32][C@H:7]1[NH:8][C:5](=[O:4])[C@H:6]1[NH:10][C:11]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)(=[O:33])[CH3:31]

参加物

5

反応物 2

HCID 23670855Potassium ethanethioateHCID 53918863HCID 53918863、化合物

生成物 1

HCID 54147731HCID 54147731、化合物収率 26.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 0.7 g of (3S,4S)-4-acetoxy-3-tritylamino-2-oxoazetidine in 10 ml of methanol is added a solution of 0.25 g of potassium thioacetate in 2 ml of water. The mixture is stirred for 30 minutes at 55°-60° C. Methanol is distilled off under reduced pressure. To the residue is added ethyl acetate, followed by washing with water, drying and concentration under reduced pressure. The residue is purified on a silica-gel column (ethyl acetate:n-hexane=1:1) to give 0.195 g of (3R,4R)-4-acetylthio-3-tritylamino-2-oxoazetidine

後処理

  1. distillationMethanol is distilled off under reduced pressure
  2. additionTo the residue is added ethyl acetate
  3. washby washing with water
  4. customdrying
  5. concentrationconcentration 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-566aa6bb78b345cf8c67e3ee3700f4b8
出典データセット
uspto-grants-1989_04
特許番号
US04822788

反応ノート

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