Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic anhydride → Tert-butyl 2-cyano-4,4-difluoropiperidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic anhydride | HCID 9845 | — |
| 반응물 | Tert-butyl 2-carbamoyl-4,4-difluoropiperidine-1-carboxylate | HCID 67286514 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Sodium Bicarbonate | HCID 516892 | — |
| 생성물 | Tert-butyl 2-cyano-4,4-difluoropiperidine-1-carboxylate | HCID 67284864 | — |
반응 단계
To a solution of tert-butyl 2-carbamoyl-4,4-difluoro-piperidine-1-carboxylate, 13g, (1.72 g, 6.51 mmol) in CH2Cl2 (50 mL) was added was N,N-triethylamine (2.03 mL, 14.61 mmol) followed by the dropwise addition of (2,2,2-trifluoroacetyl)-2,2,2-trifluoroacetate (1.02 mL, 7.32 mmol). After 15 minutes, the mixture was diluted with aqueous saturated NaHCO3 solution and the layers were separated. The organic phase was washed with water, dried over Na2SO4, filtered and evaporated to dryness. The crude residue was passed through a plug of silica gel and eluted with 10-30% EtOAc/hexanes to afford the desired product, 13h.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08829007B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-c409c9554e0042f3a22511bb23544bf9 |
| 출처 메모 | uspto-grants-2014_09 |