Hydrochloric Acid → beta-Chlorocinnamoyl chloride

HRID 1089054노트

반응식

HRID 1089054 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 54043414beta-Chlorocinnamoyl chloride수율 86%

시약·촉매·용매 1

HCID 24387Phosphorus trichloride용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f4f4670f56214e268cfebad9975c00f4
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04964896

반응 노트

불러오는 중…