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

HRID 980268

반응식

HRID 980268 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 물질

4

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. filtrationThe solids are then suction-filtered whilst hot,
  2. washwashed with acetonitrile
  3. concentrationthe filtrate is concentrated by evaporation in vacuo
  4. customThe oil remaining crystallises when
  5. waitleft
  6. customis recrystallised from 320 ml of ethyl acetate, with carbon treatment

출처 및 근거

ORD 기록
ord-b1d63c5260a54f99ba2c099d46816c80
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04636511

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