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Ammonium Hydroxide → 3-(2-Chloro-6-methylphenoxy)-1-azetidinecarboxamide

HRID 2371744
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반응식

HRID 2371744 반응식
[Cl:1][C:2]1[CH:15]=[CH:14][CH:13]=[C:12]([CH3:16])[C:3]=1[O:4][CH:5]1[CH2:8][N:7]([C:9](Cl)=[O:10])[CH2:6]1.[OH-].[NH4+:18]>O1CCCC1.O>[Cl:1][C:2]1[CH:15]=[CH:14][CH:13]=[C:12]([CH3:16])[C:3]=1[O:4][CH:5]1[CH2:8][N:7]([C:9]([NH2:18])=[O:10])[CH2:6]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 150422313-(2-Chloro-6-methylphenoxy)-1-azetidinecarbonyl chloride

생성물 1

HCID 199062253-(2-Chloro-6-methylphenoxy)-1-azetidinecarboxamide수율 77.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A stirred solution of 3.9 g (0.015 mole) of 3-(2-chloro-6-methylphenoxy)-1-azetidinecarbonyl chloride in 20 mL of tetrahydrofuran was treated all at once with 2.8 mL (0.045 mole) of 57% ammonium hydroxide. After stirring for 72 h the reaction mixture was diluted with 200 mL of water and the precipitated product collected by filtration (3.6 g of pale yellow product). Recrystallization from benzene yielded 2.8 g (69.2%) of fine white crystals, mp 256°-157° C.

후처리

  1. filtrationthe precipitated product collected by filtration (3.6 g of pale yellow product)
  2. customRecrystallization from benzene

출처 및 근거

ORD 기록
ord-a146e8d89a734345986151fd9987599c
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05095014

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