関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylamine | HCID 6341 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 8-Bromo-6-chloro-N-(3-fluoropyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide | HCID 59624495 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 6-chloro-8-(ethylamino)-N-(3-fluoropyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide | HCID 59624729 | 76.6% |
反応手順
A suspension of 5A (80 mg, 0.245 mmol), ethanamine (0.6 mL, 1.200 mmol, 2 M/THF) and DIEA (0.086 mL, 0.491 mmol) in NMP (0.7 mL) was heated at 80° C. for 5 h. The reaction mixture was cooled to room temperature and the solid was collected by filtration and washed with a small amount of DCM to give 6-chloro-8-(ethylamino)-N-(3-fluoropyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide as a yellow solid 62.8 mg. HPLC Rt=2.517 minutes (Chromolith SpeedROD 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA, 4 min gradient, monitored at 220 nm). [M+H]=335.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08389527B2 |
|---|
| 出典データセット | uspto-grants-2013_03 |
|---|
| ORD ID | ord-cd8ca855d28f4b5782930fb07458e03c |
|---|
| 出典メモ | uspto-grants-2013_03 |
|---|