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4-Chlorobenzenesulfonyl chloride → tert-butyl (2R)-2-{[(4-chlorophenyl)sulfonyl]amino}propanoate

HRID 1892832
ノート
印刷プレビュー

反応式

HRID 1892832 の反応式
Cl.[C:2]([O:6][C:7](=[O:11])[C@@H:8]([CH3:10])[NH2:9])([CH3:5])([CH3:4])[CH3:3].C(N(CC)CC)C.[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([S:26](Cl)(=[O:28])=[O:27])=[CH:22][CH:21]=1>C(Cl)Cl>[Cl:19][C:20]1[CH:25]=[CH:24][C:23]([S:26]([NH:9][C@H:8]([CH3:10])[C:7]([O:6][C:2]([CH3:5])([CH3:4])[CH3:3])=[O:11])(=[O:28])=[O:27])=[CH:22][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 8471TriethylamineHCID 16211919D-Alanine tert-butyl ester hydrochloride

生成物 1

HCID 66934865tert-butyl (2R)-2-{[(4-chlorophenyl)sulfonyl]amino}propanoate収率 88.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To D-alanine tert-butyl ester hydrochloride (1 g) in methylene chloride (35 ml) solution, triethylamine (1.7 ml) and 4-chlorobenzenesulfonyl chloride (1.1 g) were added under ice cooling and the mixture was stirred at room temperature for 2 hours. The methylene chloride was distilled off in vacuo, then the residue was diluted with ethyl acetate. The obtained solution was successively washed with distilled water, saturated potassium hydrogensulfate aqueous solution, and saturated saline, dried over with anhydrous sodium sulfate, then concentrated. The residue was recrystallized from ethyl acetate/hexane to obtain the title compound (1.47 g).

後処理

  1. distillationThe methylene chloride was distilled off in vacuo
  2. additionthe residue was diluted with ethyl acetate
  3. washThe obtained solution was successively washed with distilled water, saturated potassium hydrogensulfate aqueous solution, and saturated saline
  4. dry with materialdried over with anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-1b4d028194824a52bbf206e10939c0b3
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507714B2

反応ノート

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