Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic acid → 5-Cyano-3-methylpyridine-2-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | 1,3-Dimethoxybenzene | HCID 9025 | — |
| 반응물 | 5-Cyano-3-methyl-pyridine-2-carboxylic acid tert-butyl ester | HCID 66665826 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 5-Cyano-3-methylpyridine-2-carboxylic acid | HCID 66665846 | — |
반응 단계
To a solution of 8.50 g (38.9 mmol) 5-cyano-3-methyl-pyridine-2-carboxylic acid tert-butyl ester in 51 ml (389 mmol) 1,3-dimethoxybenzene were added 85 ml TFA and stirred for 6.5 h. The reaction mixture was diluted with toluene and evaporated. The residue was taken up in toluene and evaporated (2×). The product was crystallized from TBME/hexanes to give the title compound as a white powder. HPLC: RtH1=2.314 min; ESIMS [M+Na]+=163; 1H-NMR (360 MHz, CDCl3): δ 8.77 (s, 1H), 8.07 (s, 1H), 2.87 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524897B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-d190e2cba5834572b06ba6de8bb7dcc5 |
| 출처 메모 | uspto-grants-2013_09 |