1-Chloroethyl chloroformate → Azetidin-3-yl(4-chlorophenyl)methanone hydrochloride

HRID 1182087ノート

反応式

HRID 1182087 の反応式
C([N:14]1[CH2:17][CH:16]([C:18]([C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=2)=[O:19])[CH2:15]1)(C1C=CC=CC=1)C1C=CC=CC=1.ClC(OC(Cl)=O)C>ClCCl>[ClH:26].[NH:14]1[CH2:17][CH:16]([C:18]([C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=2)=[O:19])[CH2:15]1

参加物

4

反応物 2

HCID 5213051-Chloroethyl chloroformateHCID 69361102(1-Benzhydryl-azetidin-3-yl)-(4-chloro-phenyl)-methanone

生成物 1

HCID 69358091Azetidin-3-yl(4-chlorophenyl)methanone hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of (1-Benzhydryl-azetidin-3-yl)-(4-chloro-phenyl)-methanone (19.8 g, 54.8 mmol) in dichloromethane (250 ml), cooled to −4° C., is treated with 1-chloroethylchloroformate (8.0 ml, 73.8 mmol) and allowed to warm to ambient temperature. The reaction mixture is stirred for 18 hours and then evaporated. The residue is dissolved in methanol (220 ml) and stirred at ambient temperature for 3.5 hours. The methanol solution is concentrated and the product precipitated by addition of diethylether. The precipitate is collected by filtration and dries under high vacuum to afford Azetidin-3-yl-(4-chloro-phenyl)-methanone hydrochloride. [MH]+ 195.95.

後処理

  1. customevaporated
  2. dissolutionThe residue is dissolved in methanol (220 ml)
  3. stirringstirred at ambient temperature for 3.5 hours
  4. concentrationThe methanol solution is concentrated
  5. customthe product precipitated by addition of diethylether
  6. filtrationThe precipitate is collected by filtration and dries under high vacuum

出典と根拠

ORDレコード
ord-650a3f69dbc245e8888a830ff0612043
出典データセット
uspto-grants-2007_10
特許番号
US07288537B2

反応ノート

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