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Epichlorohydrin → N-[2-(2,3-epoxypropoxy)benzyl]-N'-(2-hydroxyethyl)urea

HRID 4538
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반응식

HRID 4538 반응식
[OH:1][CH2:2][CH2:3][NH:4][C:5]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[OH:15])=[O:6].C(=O)([O-])[O-].[K+].[K+].[CH2:22]([CH:24]1[O:26][CH2:25]1)Cl>>[O:26]1[CH2:25][CH:24]1[CH2:22][O:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[CH2:8][NH:7][C:5]([NH:4][CH2:3][CH2:2][OH:1])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 7835EpichlorohydrinHCID 11430Potassium CarbonateHCID 13754438N-(2-hydroxyethyl)-N'-(2-hydroxybenzyl)urea

생성물 1

HCID 13754439N-[2-(2,3-epoxypropoxy)benzyl]-N'-(2-hydroxyethyl)urea

실험 절차

A mixture of 29.2 g of N-(2-hydroxyethyl)-N'-(2-hydroxybenzyl)urea, 440 ml of epichlorohydrin and 38.9 g of potassium carbonate is stirred for 6 hours at 90°. The solids are then suction-filtered whilst hot, washed with acetonitrile and the filtrate is concentrated by evaporation in vacuo. The oil remaining crystallises when left to stand and is recrystallised from 320 ml of ethyl acetate, with carbon treatment. The resulting epoxide melts at 96°-99°.

후처리

  1. filtration
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
The solids are then suction-filtered whilst hot,
  • washwashed with acetonitrile
  • concentrationthe filtrate is concentrated by evaporation in vacuo
  • customThe oil remaining crystallises when
  • waitleft
  • customis recrystallised from 320 ml of ethyl acetate, with carbon treatment
  • 출처 및 근거

    ORD 기록
    ord-b83de7ddf3984ec7810453a88a6980b1
    출처 데이터셋
    uspto-grants-1988_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04727067

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