Acetic Anhydride → 2-Methylpropyl 2-cyano-3-ethoxyprop-2-enoate

HRID 1980219노트

반응식

HRID 1980219 반응식
[C:1]([CH2:3][C:4]([O:6][CH2:7][CH:8]([CH3:10])[CH3:9])=[O:5])#[N:2].[C:11]([O:14][C:15](=O)C)(=O)[CH3:12].C(OCC)(OCC)OCC>>[C:1]([C:3](=[CH:15][O:14][CH2:11][CH3:12])[C:4]([O:6][CH2:7][CH:8]([CH3:10])[CH3:9])=[O:5])#[N:2]

참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 25918Isobutyl cyanoacetateHCID 31214Ethyl orthoformate

생성물 1

HCID 537568292-Methylpropyl 2-cyano-3-ethoxyprop-2-enoate

실험 절차

A mixture of isobutyl cyanoacetate (30 g), acetic anhydride (58 ml) and triethyl orthoformate (43 ml) was heated under reflux for 6 hours. The volatile material was evaporated and the residue was distilled to give isobutyl 2-cyano-3-ethoxy-2-propenoate, b.p. 130°-133° C./0.4 mm. A solution of this (6 g) in ethanol (30 ml) was mixed with benzylmethylamine (4 ml). The mixture was heated under reflux for 10 minutes and then cooled and diluted with water (50 ml). The solid was filtered and recrystallised from ethanol giving isobutyl 3-(benzylmethylamino)-2-cyano-2-propenoate, mp 105°-106° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. customThe volatile material was evaporated
  4. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-55405d428a034e609ccfb9bd77590936
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04508659

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