Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Aminophenol → 4-(1,1-Difluoro-2,2,2-trichloroethoxy)aniline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Aminophenol | HCID 403 | — |
| 반응물 | 1,1,1,2-Tetrachloro-2,2-difluoroethane | HCID 6426 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 4-(1,1-Difluoro-2,2,2-trichloroethoxy)aniline | HCID 13529255 | — |
반응 단계
2.0 g (18.3 mmol) of p-aminophenol was added over a period of 10 minutes to a mixture of 0.48 g (20.1 mmol) of sodium hydride in 20 ml of dry DMSO. The mixture was stirred for 20 minutes. 3.73 g (18.3 mmol) of 1,1-difluoro-tetrachloroethane was added causing an exotherm to 47° C. The mixture was stirred at 60° C. for 2 hours, then poured into ice water. The brown solid was collected by filtration, dried, dissolved in ether and then HCl gas was bubbled into the solution causing the above-named aniline to precipitate as the hydrochloride salt. The white solid (4.4 g, 87 percent of theoretical d 250° C.) was collected by filtration.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05250690 |
| 출처 데이터셋 | uspto-grants-1993_10 |
| ORD ID | ord-ce4291de36e44412b9bd74ae5712ae97 |
| 출처 메모 | uspto-grants-1993_10 |