化工社化工社 化学情報印刷レポート · 研究参考用
Phosphorus oxychloride → 7-Bromo-1-chloro-6-methoxyisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 7-Bromo-6-methoxy-1(2H)-isoquinolinone | HCID 58005125 | — |
| 生成物 | 7-Bromo-1-chloro-6-methoxyisoquinoline | HCID 59571146 | — |
反応手順
A mixture of the product from Step 2 (7-bromo-6-methoxyisoquinolin-1(2H)-one) (4.7 g, 18.5 mmol) in phosphorus oxychloride (30 mL) was heated to reflux for 2 hours and cooled to RT. The volatiles were then evaporated, and the residue was partitioned between 3 M NaOH and DCM. The organic phase was dried over Na2SO4; the solvent was evaporated; and the solid was triturated with Et2O (20 mL) and filtered to give a solid (3.75 g). LRMS ESI+ (M+H)+274.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08138164B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-1c7f084ad557447b9e4b7da6550e61c7 |
| 出典メモ | uspto-grants-2012_03 |