참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | (2-Thienylmethyl)amine | HCID 34005 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Chloro-6-methylnicotinic acid | HCID 121724 | — |
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | Ethyl acetate hexane | HCID 21226206 | — |
| 생성물 | 2-chloro-6-methyl-N-(thiophen-2-ylmethyl)nicotinamide | HCID 86628836 | 63% |
반응 단계
2.67 g (7.0 mmol) of HATU and 4.0 ml (23.2 mmol) of DIPEA were added at 0° C. to a solution of 1.0 g (5.8 mmol) of 2-chloro-6-methyl-nicotinic acid in DMF (20 ml), and the mixture was stirred for 20 min at 0° C. At that temperature, 656 mg (5.8 mmol) of thiophen-2-ylmethylamine were added. Stirring was then carried out for 16 h at RT. The mixture was then diluted with EA and washed in succession with sat. aq. NaHCO3 solution and brine. The organic phase was dried over Na2SO4, filtered and concentrated in vacuo. CC (hexane/EA 4:1) of the residue yielded 966 mg (3.6 mmol, 63%) of 2-chloro-6-methyl-N-(thiophen-2-ylmethyl)nicotinamide.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08084470B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_12 |
|---|
| ORD ID | ord-576134ea9a1c469596421bcd43466380 |
|---|
| 출처 메모 | uspto-grants-2011_12 |
|---|
