Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetonitrile → N-(6-Chloro-3-pyridylmethyl)-N-(2,2,2-trifluoroethyl)amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,2,2-Trifluoroethylamine hydrochloride | HCID 9772 | — |
| 반응물 | 2-Chloro-5-(chloromethyl)pyridine | HCID 155479 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N-(6-Chloro-3-pyridylmethyl)-N-(2,2,2-trifluoroethyl)amine | HCID 22450432 | 92.7% |
반응 단계
In 15 ml of water was dissolved 12.55 g of 2,2,2-trifluoroethylamine hydrochloride, followed by addition of 68 ml of CH3CN, and further 9.35 g of Et3N and then 3.00 g (0.0185 mole) of 6-chloro-3-pyridylmethyl chloride under cooling with ice-water and stirring. The mixture was stirred at room temperature for one hour, at 50° C. for one hour and at 70° C. for 90 hours. The CH3CN was distilled off, and the residue was followed by addition of NaHCO3 and then extracted with CH2Cl2 (100 ml×3). The extract was dried over MgSO4 and distilled to remove CH2Cl2. To the residue was added 100 ml of Et2O and the resulting unsoluble matter was filtered off. The filtrate was concentrated to give 3.85 g of the title compound as yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05214152 |
| 출처 데이터셋 | uspto-grants-1993_05 |
| ORD ID | ord-1156530060f14c9587f7dd9fd59c4597 |
| 출처 메모 | uspto-grants-1993_05 |