Water → HCID 23289323、化合物

HRID 366458ノート

反応式

HRID 366458 の反応式
[C:1]([O:4][C:5]1[C:10]2[CH2:11][CH2:12][CH2:13][C:14](=[S:16])[NH:15][C:9]=2[CH:8]=[CH:7][CH:6]=1)(=[O:3])[CH3:2].F[B-](F)(F)F.[CH3:22][O+](C)C.O>C(Cl)Cl>[C:1]([O:4][C:5]1[C:10]2[CH2:11][CH2:12][CH2:13][C:14]([S:16][CH3:22])=[N:15][C:9]=2[CH:8]=[CH:7][CH:6]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 962WaterHCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 23289285HCID 23289285、化合物

生成物 1

HCID 23289323HCID 23289323、化合物収率 91.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1,3,4,5-tetrahydro-6-acetoxy-2H-1-benzazepin-2-thione (235 mg, 1.0 mmol) in 25 mL of CH2Cl2 was added at 0° 295 mg (2.0 mmol) of trimethyloxonium tetrafluoroborate. After stirring at room temperature for about 30 min. water was added and the CH2Cl2 layer was separated. Drying over Na2SO4 and removal of the solvent gave 229 mg of 4,5-dihydro-6-acetoxy-2-methylthio-3H-benzazepine.

後処理

  1. additionwas added
  2. customthe CH2Cl2 layer was separated
  3. dry with materialDrying over Na2SO4 and removal of the solvent

出典と根拠

ORDレコード
ord-3b8f0b3662d84939ba864cec54953c2d
出典データセット
uspto-grants-2000_10
特許番号
US06130217

反応ノート

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