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1,3-Dimethyl-2-imidazolidinone → 4-Butylamino-2-chloro-6-nitroquinazoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Dimethyl-2-imidazolidinone | HCID 6661 | — |
| 反応物 | Butylamine | HCID 8007 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 6-Nitro-2,4(1H,3H)-quinazolinedione | HCID 816982 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Butylamino-2-chloro-6-nitroquinazoline | HCID 18326426 | 63.6% |
反応手順
To 500 mg (2.41 mmol) of 6-nitroquinazoline-2,4 (1H,3H)-dione were added 2 ml of 1,3-dimethyl-2-imidazolidinone and 8.23 g (53.64 mmol) of phosphorus oxychloride, and the resulting mixture was subjected to heating under reflux for 3 hours. After phosphorus oxychloride was removed in vacuo, the mixture was dissolved in 5 ml of acetonitrile, followed by addition of 5.9 ml (60 mmol) of butylamine 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 430 mg (yield: 63.6%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06339089B2 |
| 出典データセット | uspto-grants-2002_01 |
| ORD ID | ord-3143ca3b790840ec8a68b2398665282c |
| 出典メモ | uspto-grants-2002_01 |