関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diethylphosphorylcyanide | HCID 13586794 | — |
| 反応物 | (3-oxo-5H-thiazolo[2,3-b]quinazolin-2(3H)-ylidene)acetic acid | HCID 54200705 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Benzene ethyl acetate | HCID 21583983 | — |
| 生成物 | N-Benzyl-(3-oxo-5H-thiazolo[2,3-b]quinazolin-2(3H)-ylidene)acetamide | HCID 54292886 | — |
反応手順
To a stirred mixture of (3-oxo-5H-thiazolo[2,3-b]quinazolin-2(3H)-ylidene)acetic acid (10.5 g, 1.9 mmols) and benzylamine (0.23 g, 2.1 mmols) in 25 ml dimethylformamide at 0° C., was added diethylphosphoryl cyanide (0.28 g, 2.1 mmols) (in dimethylformamide solution), followed by triethylamine (0.41 g, 4.0 mmols). The reaction mixture was stirred for 4 hours at 0° C. and then, at room temperature overnight. The reaction mixture was diluted with benzene-ethyl acetate and washed sequentially with 5% hydrochloric acid, water, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride. The organic solution was dried over anhydrous magnesium sulfate, and evaporated to dryness under reduced pressure to give N-Benzyl-(3-oxo-5H-thiazolo[2,3-b]quinazolin-2(3H)-ylidene)acetamide which was recrystallized from ethyl acetate. Yield--0.09 g. Mp 258°-259° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04588812 |
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| 出典データセット | uspto-grants-1986_05 |
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| ORD ID | ord-cf5698ff7a884e97b278358b34d4f565 |
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| 出典メモ | uspto-grants-1986_05 |
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