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

HRID 980268

反応式

HRID 980268 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-b1d63c5260a54f99ba2c099d46816c80
出典データセット
uspto-grants-1987_01
特許番号
US04636511

関連ノート

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