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Sodium Hydroxide → 6-Methyl-7-methoxy-1-[2-(4-chlorophenyl)ethyl]-3,4-dihydroisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | Chlorine monoxide | HCID 24646 | — |
| 反応物 | N-[2-(3-methyl-4-methoxyphenyl)ethyl]-3-(4-chlorophenyl)propionamide | HCID 19892235 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 6-Methyl-7-methoxy-1-[2-(4-chlorophenyl)ethyl]-3,4-dihydroisoquinoline | HCID 19739693 | 52.3% |
反応手順
Heat a mixture of the amide from step A (10.0 g), phosphorous pentoxide (25 g), phosphorour oxychloride (15 mL) and xylene (250 mL) at reflux for 2 h. Cool the reaction mixture, slowly add water (500 mL), basify using NaOH and extract with benzene. Concentrate the benzene extract to a residue and triturate with diethyl ether to give 6-methyl-7-methoxy-1-[2-(4-chlorophenyl)ethyl]-3,4-dihydroisoquinoline (4.95 g), mp=122°-124° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05238935 |
| 出典データセット | uspto-grants-1993_08 |
| ORD ID | ord-d5c28f1783ed4b8ba8aed73dd5022a84 |
| 出典メモ | uspto-grants-1993_08 |