Acetic Anhydride → 2-(p-Fluorobenzoyl)-3-ethoxycrotononitrile

HRID 128169

反応式

HRID 128169 の反応式
[F:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([CH2:8][C:9]#[N:10])=[O:7])=[CH:4][CH:3]=1.[C:13](OCC)(OCC)([O:15][CH2:16][CH3:17])[CH3:14].C(OC(=O)C)(=O)C>>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:6](/[C:8](=[C:13](/[O:15][CH2:16][CH3:17])\[CH3:14])/[C:9]#[N:10])=[O:7])=[CH:11][CH:12]=1

参加物

4

反応物 3

HCID 7918Acetic AnhydrideHCID 66221Triethyl orthoacetateHCID 2783172p-Fluorobenzoylacetonitrile

生成物 1

HCID 705293312-(p-Fluorobenzoyl)-3-ethoxycrotononitrile

実験手順

A solution of 16.3 g. of p-fluorobenzoylacetonitrile and 18.3 ml. of triethyl orthoacetate in 35 ml. of acetic anhydride is heated on a steam bath for 2.5 hours. The solvents are removed in vacuo and the residue is distilled at 165°-167° C./300μ. Upon cooling, this distillate solidifies and is recrystallized from methylene chloride/hexane to give the desired 2-(p-fluorobenzoyl)-3-ethoxycrotononitrile, m.p. 77°/89° C.

後処理

  1. customThe solvents are removed in vacuo
  2. distillationthe residue is distilled at 165°-167° C./300μ
  3. temperatureUpon cooling
  4. customthis distillate solidifies and is recrystallized from methylene chloride/hexane

出典と根拠

ORDレコード
ord-ea48427f139844aca6b6b4feacd5221b
出典データセット
uspto-grants-1981_03
特許番号
US04259256

関連ノート

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