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Sulfuric Acid → 7,8-Dimethoxy-2-methyl-3H-pyrimido[4,5-b]quinolin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Amino-6,7-dimethoxyquinoline-3-carboxamide | HCID 781584 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 7,8-Dimethoxy-2-methyl-3H-pyrimido[4,5-b]quinolin-4-one | HCID 135822648 | — |
反応手順
Concentrated sulfuric acid (1.5 ml.) is added to a slurry of 6,7-dimethoxy-2-aminoquinoline-3-carboxamide (5.0 g., 0.02 mole) and acetic anhydride (40 ml.) The slurry dissolves to give a dark orange solution from which a heavy yellow precipitate separates. Acetic anhydride (10 ml.) is added to facilitate stirring and heating continued for an additional 75 minutes. The mixture is cooled, water (50 ml.) added and the resulting solution made alkaline with 5N sodium hydroxide (225 ml.). It is chilled, the precipitate collected by filtration and air-dried. The yellow solid is recrystallized from ethanol. Yield = 2.37 g., M.P. 300°-302° (dec.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04044134 |
| 出典データセット | uspto-grants-1977_08 |
| ORD ID | ord-c5c625fdaf0245468c39c734208518d5 |
| 出典メモ | uspto-grants-1977_08 |