Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic acid → 5-(5-(3-Hydroxy-3-methylbut-1-ynyl)-4-(piperidin-4-ylmethylamino)pyridin-2-ylamino)pyrazine-2-carbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | tert-Butyl 4-((2-(5-cyanopyrazin-2-ylamino)-5-(3-hydroxy-3-methylbut-1-ynyl)pyridin-4-ylamino)methyl)piperidine-1-carboxylate | HCID 59613530 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-(5-(3-Hydroxy-3-methylbut-1-ynyl)-4-(piperidin-4-ylmethylamino)pyridin-2-ylamino)pyrazine-2-carbonitrile | HCID 59613386 | 50% |
반응 단계
TFA (0.2 mL) was added at room temperature to a solution of tert-butyl 4-((2-(5-cyanopyrazin-2-ylamino)-5-(3-hydroxy-3-methylbut-1-ynyl)pyridin-4-ylamino)methyl)piperidine-1-carboxylate (0.020 g, 0.041 mmol) dissolved in dichloromethane (2 mL). The reaction mixture was stirred for 20 min. Solvent was removed in vacuo and the crude mixture was purified by ion exchange on SCX-II acidic resin (500 mg), eluting with methanol then 2M ammonia-methanol. The basic fractions were combined and solvent was removed in vacuo. The crude product was purified by preparative thin layer chromatography, eluting with methanol/dichloromethane (1/19), to give the title compound as a yellow solid (0.008 g, 50%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08058045B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-129bc5d8ac80425eb5e31c0cf4c34ff7 |
| 출처 메모 | uspto-grants-2011_11 |