Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2-Hydroxy-3-methyl-2-(trifluoromethyl)butan-1-aminium chloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 1,1,1-Trifluoro-3-methyl-2-(nitromethyl)butan-2-ol | HCID 86657673 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-Hydroxy-3-methyl-2-(trifluoromethyl)butan-1-aminium chloride | HCID 86657674 | — |
반응 단계
To a solution of 1,1,1-trifluoro-3-methyl-2-(nitromethyl)butan-2-ol (753 mg, 3.74 mmol) in EtOH (10 ml) in a 25 ml medium pressure glass hydrogenation vessel under N2, 10% Pd on carbon (39.8 mg, 0.374 mmol) was added. The vessel was flushed with N2, followed by H2 (22.64 mg, 11.23 mmol) at 5 bar pressure and stirred at RT for 6 days. The mixture was filtered through Celite® and washed through with EtOH (30 ml), followed by DCM (10 ml). The filtrate was concentrated under vacuum to give a colourless oil. The crude product was taken up in methanol (20 ml) and treated with a 1.25M HCl in methanol solution. The resulting colourless solution was stirred at RT for 1 hour and concentrated under vacuum to afford the title compound;
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08476269B2 |
| 출처 데이터셋 | uspto-grants-2013_07 |
| ORD ID | ord-03e54ff895854bf6b5120f25a44ac2f0 |
| 출처 메모 | uspto-grants-2013_07 |