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Ethyl chloroformate → 2-hydroxy-3-[3-(1H-imidazol-1-yl)propyl]quinazolin-4(3H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 2-amino-N-(3-imidazol-1-ylpropyl)benzamide | HCID 2798335 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-hydroxy-3-[3-(1H-imidazol-1-yl)propyl]quinazolin-4(3H)-one | HCID 13952769 | — |
反応手順
A mixture of 4.0 g of 2-amino-N-[3-(1H-imidazol-1-yl)propyl]benzamide and 15 ml of ethyl chloroformate was heated in an oil bath at 95°-105° C. for 1.5 hours, dissolved in 50 ml of ethanol, and concentrated. The residue was mixed with 100 ml of ethanol and 3.2 g of potassium hydroxide, heated at reflux temperature for 3 hours and concentrated. The residue was dissolved in water and acidified with acetic acid to pH 6-7. The white precipitate was separated by filtration and recrystallized from ethanol. The desired product melted at 197°-200° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04684654 |
| 出典データセット | uspto-grants-1987_08 |
| ORD ID | ord-e6e5308386f14afbbdcf8015ffa02749 |
| 出典メモ | uspto-grants-1987_08 |