関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-[2-(3,4-dimethoxyphenyl)ethyl]formamide | HCID 84337 | — |
| 溶媒 | Ammonia | HCID 222 | — |
| 生成物 | 3,4-Dihydro-6,7-dimethoxyisoquinoline | HCID 30058 | — |
反応手順
The N-formyl-2(3,4-dimethoxy-phenyl)-ethylamine so obtained is stirred with polyphosphoric acid (1 kg) and heated to 140° C. (oil bath temperature). The reaction mixture foams vigorously starting from an internal temperature of 70° C. After 30 minutes, an internal temperature of about 140° C. is attained. The mixture is then poured onto water (1 liter) and made alkaline with concentrated ammonia (1.8 liters) while ice is added. The reaction product is extracted repeatedly with ethyl acetate, the ethyl acetate phase is washed with water, dried, over magnesium sulphate and evaporated giving the title compound (142.5 g) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04678792 |
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| 出典データセット | uspto-grants-1987_07 |
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| ORD ID | ord-6d8dbedc0f774882852ce542ea9e0af5 |
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| 出典メモ | uspto-grants-1987_07 |
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