関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | ethyl 2-(8-(benzo[d]thiazol-2-ylcarbamoyl)-3,4-dihydroisoquinolin-2(1H)-yl)-5-(3-iodopropyl)thiazole-4-carboxylate | HCID 59447467 | — |
| 反応物 | tert-butyl 5-amino-4-cyano-3-(4-hydroxyphenyl)-1H-pyrazole-1-carboxylate | HCID 136027725 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178509393 | HCID 178509393 | — |
反応手順
To compound 31F (0.132 g, 0.44 mmol) in DMF (4 mL) was added 60% sodium hydride (0.048 g, 1.2 mmol) at 0° C. The solution was stirred for 10 minutes. To this solution was added compound 2C. The solution was stirred at rt for 2 hours. The solution was diluted with conc. HCl (0.5 mL), and heated at 60° C. for 30 minutes. The mixture was diluted with DMSO (5 mL) and MeOH (9 mL). The solid was filtered off. The filtrate was then purified by Prep HPLC to provide 12 mg of the desired product: 1H NMR (DMSO-d6): δ 8.03 (d, J=7.98 Hz, 1H), 7.79 (d, J=7.98 Hz, 1H), 7.67-7.71 (m, 4H), 7.33-7.49 (m, 5H), 7.00 (d, J=8.59 Hz, 2H), 4.84 (s, 2H), 4.03 (t, J=5.98 Hz, 2H), 3.71-3.74 (m, 2H), 3.17-3.20 (m, 2H), 3.01-3.05 (m, 2H), 2.02 (m, 2H). MS (ESI(+)): 677 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08232273B2 |
|---|
| 出典データセット | uspto-grants-2012_07 |
|---|
| ORD ID | ord-9b5d6183273046099c1cc16e837531f2 |
|---|
| 出典メモ | uspto-grants-2012_07 |
|---|
