Hydrochloric Acid → 2-Chloro-1-(2,4-difluorophenyl)ethanone

온도

0 °C

Into the solution of 1,3-difluorobenzene in 1,2-dicholoroethane (DCE) was added anhydrous aluminium chloride (1.2 molar equivalent of 1,3-difluorobenzene) at 25-30° C. and stirred for 30 minutes. The reaction mixture was then cooled to 0° C. and chloroacetyl chloride (1.1 molar equivalent of 1,3-difluorobenzene), in DCE, was then added into it over a period of 30-60 min keeping the reaction temperature below 20° C. After the addition was over, the reaction mixture was stirred at 25-30° C. for 5-7 hours. The reaction mixture was then diluted with DCE and poured into dil. hydrochloric acid (5%) at 0-5° C. The mixture was then extracted with DCE. The combined organic layer was washed successively with 5% aq. sodium bicarbonate solution and water. Evaporating DCE from the organic layer under reduced pressure gave an oil which on triturating with n-Hexane gave the title compound as white crystalline material (Yield 75% of theory).

1. customthe reaction temperature below 20° C
2. additionAfter the addition
3. stirringwas stirred at 25-30° C. for 5-7 hours
4. extractionThe mixture was then extracted with DCE
5. washThe combined organic layer was washed successively with 5% aq. sodium bicarbonate solution and water
6. customEvaporating DCE from the organic layer under reduced pressure gave an oil which
7. customon triturating with n-Hexane

ORD 기록

ord-186f0a5f3da4434294b577da0c0bf1d7

출처 데이터셋

uspto-grants-2003_12

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06670363B1