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

HRID 4538

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 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-b83de7ddf3984ec7810453a88a6980b1
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727067

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