Ethanol → Benzoic acid, 2,4-dichloro-5-fluoro-, ethyl ester

반응식

[Cl:1][C:2]1[CH:10]=[C:9]([Cl:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH2:13]([OH:15])[CH3:14]>>[Cl:1][C:2]1[CH:10]=[C:9]([Cl:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([O:15][CH2:13][CH3:14])=[O:5]

참가 물질

반응물 2

HCID 702Ethanol

HCID 27368212,4-Dichloro-5-fluorobenzoyl chloride

생성물 1

HCID 13630722Benzoic acid, 2,4-dichloro-5-fluoro-, ethyl ester수율 97%

실험 절차

84 g of 2,4-dichloro-5-fluoro-benzoyl chloride are added dropwise to 250 ml of anhydrous ethanol at 50° to 60° C., the temperature being maintained by occasional cooling with ice-water. The mixture is then refluxed for about a further hour, the excess alcohol is distilled off and the residue is fractionated in vacuo. 84.9 g (~97%) of ethyl 2,4-dichloro-5-fluoro-benzoate are obtained at 132°-135° C./8 mbar.

후처리

temperaturethe temperature being maintained
temperatureThe mixture is then refluxed for about a further hour
distillationthe excess alcohol is distilled off

출처 및 근거

ORD 기록: ord-84f4a811032d4a7ea1669fb806d713ad
출처 데이터셋: uspto-grants-1991_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04990646

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