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

HRID 1182087노트

반응식

HRID 1182087 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-650a3f69dbc245e8888a830ff0612043
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07288537B2

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