Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium tert-butoxide → 4-(5-Trifluoromethyl-benzo[d]isoxazol-3-yl)-piperidine-1-carboxylic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | 4-[(2-Fluoro-5-trifluoromethyl-phenyl)-hydroxyiminomethyl]-piperidine-1-carboxylic acid tert-butyl ester | HCID 72434547 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(5-Trifluoromethyl-benzo[d]isoxazol-3-yl)-piperidine-1-carboxylic acid tert-butyl ester | HCID 58817530 | 106.1% |
반응 단계
A solution of 4-[(2-Fluoro-5-trifluoromethyl-phenyl)-hydroxyimino-methyl]-piperidine-1-carboxylic acid tert-butyl ester (4.969 g, 0.013 M) in anhydrous THF (59 mL) was treated with Potassium tert-butoxide (13.4 mL of a 1M solution in THF, 0.0133 M-1.05 eq). The mixture was stirred at ambient temperature for 1 hour and then heated to 65° C. for 2 hours. The THF was removed under reduced pressure. The residue was dissolved in ethyl acetate (100 mL), washed with H2O (50 mL) and brine (50 mL) respectively. It was then dried over MgSO4, filtered and concentrated to give a solid (5 g) which was purified on silica ˜120 g, (eluting with ethylacetate heptane (30:70) to give the product as a white solid (2.69 g, 57%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07772252B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-cc987dde104b489ab6857cf32d915e8a |
| 출처 메모 | uspto-grants-2010_08 |