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Triphenylphosphine dichloride → 7,8-Dichloro-4-methylisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine dichloride | HCID 260420 | — |
| 反応物 | HCID 21393806 | HCID 21393806 | — |
| 生成物 | 7,8-Dichloro-4-methylisoquinoline | HCID 21393849 | — |
反応手順
8-Chloro-7-hydroxy-4-methylisoquinoline (0.04 mole) and dichlorotriphenylphosphorane (0.04 mole) are heated to 240° C. under a nitrogen atmosphere. After four hours, the mixture is allowed to cool and is partitioned between chloroform and concentrated hydrochloric acid. The acidic extract is washed with chloroform, basified and extracted with chloroform. The chloroform extract is washed with water, dried over sodium sulfate and evaporated to yield 7,8-dichloro-4-methylisoquinoline. The product is purified by chromatography on silica gel eluted with chloroform and finally by precipitation of the hydrochloride from ethanol-ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04062961 |
| 出典データセット | uspto-grants-1977_12 |
| ORD ID | ord-5b22cc1d06044d2b8335d8b22366d2ad |
| 出典メモ | uspto-grants-1977_12 |