関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dodecylamine | HCID 13583 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | N,N-bis(1-methylethyl)formamide | HCID 75912 | — |
| 反応物 | 6-Nitro-2,4(1H,3H)-quinazolinedione | HCID 816982 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Chloro-4-dodecylamino-6-nitroquinazoline | HCID 18326516 | 67% |
反応手順
To 250 mg (1.21 mmol) of 6-nitroquinazoline-2,4(1H,3H)-dione were added 5.00 ml (53.64 mmol) of phosphorus oxychloride and 0.18 ml (1.21 mmol) of diisopropylformamide, and the resulting mixture was subjected to heating under reflux for 24 hours. After phosphorus oxychloride was removed in vacuo, the mixture was dissolved in 5 ml of acetonitrile, followed by addition of 2.80 ml (12.10 mmol) of dodecylamine under ice cooling and stirring under ice cooling for 30 minutes. To the reaction solution was added water, followed by extraction with ethyl acetate, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 310 mg (67.0%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06339089B2 |
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| 出典データセット | uspto-grants-2002_01 |
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| ORD ID | ord-7f8e17d78fb44cd0b29b18b84e7c2205 |
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| 出典メモ | uspto-grants-2002_01 |
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