化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → N-Cyclopropyl-3-(2-(4-hydroxybenzyl)-1-oxo-1,2-dihydroisoquinolin-6-yl)-4-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-(Chloromethyl)phenyl acetate | HCID 148312 | — |
| 反応物 | N-Cyclopropyl-4-methyl-3-(1-oxo-1,2-dihydro-isoquinolin-6-yl)-benzamide | HCID 25020457 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-Cyclopropyl-3-(2-(4-hydroxybenzyl)-1-oxo-1,2-dihydroisoquinolin-6-yl)-4-methylbenzamide | HCID 57551752 | 81.5% |
反応手順
To a solution of the product of Example 11 (460 mg) in DMF (10 mL) was added 60% sodium hydride (38 mg) and the reaction stirred at room temperature for 30 minutes before the addition of 4-(chloromethyl)phenyl acetate (280 mg). The reaction mixture was then stirred at room temperature for 17 hrs. Additional 60% sodium hydride (38 mg) was added and the reaction was stirred for a further 2 hours. NaOH (5N, 2 mL) was added and the reaction was stirred at room temperature for 90 minutes. The reaction mixture was acidified with HCl (2N) and extracted into ethyl acetate. The organics were washed with water and brine, dried over magnesium sulphate and evaporated to yield the sub-titled compound (500 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08012979B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-ab50e612b55a46608ff4714e6bba7b26 |
| 出典メモ | uspto-grants-2011_09 |