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

HRID 1980219ノート

反応式

HRID 1980219 の反応式
[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]

参加物

4

反応物 3

HCID 7918Acetic AnhydrideHCID 25918Isobutyl cyanoacetateHCID 31214Ethyl orthoformate

生成物 1

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-55405d428a034e609ccfb9bd77590936
出典データセット
uspto-grants-1985_04
特許番号
US04508659

反応ノート

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