참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Chloroacetyl chloride | HCID 6577 | — |
| 반응물 | 1,3-Difluorobenzene | HCID 9741 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 2-Chloro-1-(2,4-difluorophenyl)ethanone | HCID 588083 | 75% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06670363B1 |
|---|
| 출처 데이터셋 | uspto-grants-2003_12 |
|---|
| ORD ID | ord-186f0a5f3da4434294b577da0c0bf1d7 |
|---|
| 출처 메모 | uspto-grants-2003_12 |
|---|