Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine → 2-Chloro-6,N,N-trimethyl-isonicotinamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Chloro-6-methylpyridine-4-carboxylic acid | HCID 141209 | — |
| 반응물 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Chloro-6,N,N-trimethyl-isonicotinamide | HCID 56966855 | — |
반응 단계
To a solution of 2-Chloro-6-methyl-isonicotinic acid (1 g) in DMF (200 ml) at 25° C. was added DIPEA (2.9 mL) and TBTU (1.8 ml). After 5 min, dimethylamine (0.75 g) was added dropwise. This was stirred overnight. The reaction was added to water and extracted with EtOAc. The organic layer was separated, dried and concentrated in vacuum. Flash chromatography (9:1 to 2:8 gradient cyclohexane:EtOAc) afforded the title compound (320 mg). Rf=0.56 (1:1 cyclohexane:EtOAc)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08653075B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-70313f00a4a9493bb6a4f5a3de3d76a6 |
| 출처 메모 | uspto-grants-2014_02 |