Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic acid → (+/-)-Phenylmethyl {[cis-4-fluoro-3-pyrrolidinyl]methyl}carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | Carbonic acid--N,N-diethylethanamine (1/2) | HCID 15264167 | — |
| 반응물 | (+/-)-1,1-Dimethylethyl cis-3-fluoro-4-[({[(phenylmethyl)oxy]carbonyl}amino)methyl]-1-pyrrolidinecarboxylate | HCID 59026099 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (+/-)-Phenylmethyl {[cis-4-fluoro-3-pyrrolidinyl]methyl}carbamate | HCID 86616799 | 99.1% |
반응 단계
To a solution of (±)-1,1-dimethylethyl cis-3-fluoro-4-[({[(phenylmethyl)oxy]carbonyl}amino)methyl]-1-pyrrolidinecarboxylate (0.45 g, 1.28 mmole) in DCM (50 mL) at RT was added TFA (25 mL). After 2 h, the reaction solution was concentrated under vacuum and the residue placed under high vacuum for 3 hr. The residue was dissolved in DCM (200 mL) and MP-carbonate resin (5.12 mmole, 1.9 g) was added with vigorous stirring at RT. After 4 h, the reaction contents were filtered through a scintered-glass funnel washing with MeOH (100 mL). The filtrate was concentrated under vacuum to give the title compound (0.32 g, 99%) as a light orange oil: LC-MS (ES) m/e 253 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07691850B2 |
| 출처 데이터셋 | uspto-grants-2010_04 |
| ORD ID | ord-1546abf94dda42e5b27207a7d55e4eab |
| 출처 메모 | uspto-grants-2010_04 |