関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (2-Thienylmethyl)amine | HCID 34005 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Chloro-6-methylnicotinic acid | HCID 121724 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 2-chloro-6-methyl-N-(thiophen-2-ylmethyl)nicotinamide | HCID 86628836 | 63% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08084470B2 |
|---|
| 出典データセット | uspto-grants-2011_12 |
|---|
| ORD ID | ord-576134ea9a1c469596421bcd43466380 |
|---|
| 出典メモ | uspto-grants-2011_12 |
|---|
