Hydrochloric Acid → beta-Chlorocinnamoyl chloride

HRID 1089054ノート

反応式

HRID 1089054 の反応式
CC[O:3][C:4]([CH2:6][C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=O)=O.P(Cl)(Cl)(Cl)(Cl)[Cl:16].[ClH:21].P(Cl)(Cl)(Cl)=O>P(Cl)(Cl)Cl>[Cl:21][C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[CH:6][C:4]([Cl:16])=[O:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7170Ethyl benzoylacetateHCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachloride

生成物 1

HCID 54043414beta-Chlorocinnamoyl chloride収率 86%

試薬・触媒・溶媒 1

HCID 24387Phosphorus trichloride溶媒2 回

実験手順

A solution of 60 g (0.312 mol) ethyl benzoyl acetate in 96 ml (150 g) of phosphorous trichloride is added dropwise to 150 g(0.72 mol) of phosphorous pentachloride under nitrogen. The suspension that forms is cautiously brought to reflux temperature (HCl evolution observed) and is refluxed and stirred for 2-21/2 hrs. The solution that forms is stripped of phosphorous trichloride and phosphorous oxychloride at atmospheric pressure (76°-82° C.). The pot residue is distilled at 97°-108° C./0.75mm to give 54 g (86% yield) of product as an isomeric mixture.

後処理

  1. temperatureis refluxed
  2. distillationThe pot residue is distilled at 97°-108° C./0.75mm

出典と根拠

ORDレコード
ord-f4f4670f56214e268cfebad9975c00f4
出典データセット
uspto-grants-1990_10
特許番号
US04964896

反応ノート

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