関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Pyridinemethanamine | HCID 31018 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4,6-Dichloronicotinamide | HCID 600044 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 6-Chloro-4-(pyridin-3-ylmethylamino)nicotinamide | HCID 58440201 | 82.6% |
反応手順
A mixture of 4,6-Dichloronicotinamide (1, 950 mg, 5 mmoles), 3-picolylamine (756 mg, 7 mmoles) and DIEA (12 mmoles) in NMP (5 mL) was stirred at 60° C. for 20 hrs. The reaction mixture was concentrated under an oil pump. The residue was washed with water and dried under an oil pump. The desired 6-chloro-4-(pyridin-3-ylmethylamino)nicotinamide (2, 1.085 g) was obtained. MS+: 263.1, UV: λ=220.9; 260.9 nm. 1H NMR: (CDCl3) δ8.96 (s, 1H), δ8.60 (s, 1H), δ8.57 (d, J=3.2 Hz, 1H), δ8.30 (s, 1H), δ7.64 (d, J=7.6 Hz, 1H), δ7.31 (dd, J1=7.6 Hz, J2=3.2 Hz, 1H), δ6.51 (s, 1H), δ5.80 (b, 2H), δ4.47 (s, 1H), δ4.45 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08853230B2 |
|---|
| 出典データセット | uspto-grants-2014_10 |
|---|
| ORD ID | ord-48b153a2efb54ca08c04d192a7b26755 |
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| 出典メモ | uspto-grants-2014_10 |
|---|
