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Hydrochloric Acid → 4-Bromo-6,7-dihydro-8(5H)-isoquinolinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methyl 4-bromo-8-oxo-5,6,7,8-tetrahydroisoquinoline-7-carboxylate | HCID 86679925 | — |
| 生成物 | 4-Bromo-6,7-dihydro-8(5H)-isoquinolinone | HCID 71743380 | 69.4% |
反応手順
The crude methyl 4-bromo-8-oxo-5,6,7,8-tetrahydroisoquinoline-7-carboxylate (7.79 g, 27.4 mmol) was dissolved (small amount of not dissolved material) in aq. 6M HCl (84.1 ml, 505 mmol) and heated at reflux for 2.5 h. The acidic solution was concentrated in vacuo, suspended in water (ca. 25 mL), cooled in ice and basified with 6.0 M KOH. The aqueous solution was extracted with ether (2×) and CH2Cl2 (3×), the combined organic layers were dried over Na2SO4, filtered and concentrated to afford the title compound (4.30 g, 69%) as a brown solid. MS: 226.0 (M+H+, 1Br).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09133158B2 |
| 出典データセット | uspto-grants-2015_09 |
| ORD ID | ord-b4c0d610aadc477a800985f328480d41 |
| 出典メモ | uspto-grants-2015_09 |