関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| 反応物 | 4-Aminoquinazoline | HCID 84759 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Diethyl[(4-quinazolinylamino)methylene]propanedioate | HCID 13060467 | 90.1% |
反応手順
A mixture of 4-aminoquinazoline (11.6 g) and diethyl ethoxymethylenepropanedioate (19.0 g) in N,N-dimethylformamide (40 ml) was stirred for 1 hour and 20 minutes at 160° C. and then cooled to 0° C. to precipirate crystals. To the mixture was added small volume of water with stirring. The crystals were separated by filtration, washed with water, dried overnight under reduced pressure and dissolved in ethyl acetate. The resultant solution was dried over anhydrous magnesium sulfate and recrystallized from a mixture of ethyl acetate and hexane to give crystalline diethyl [(4-quinazolinylamino)methylene]propanedioate (22.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04377580 |
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| 出典データセット | uspto-grants-1983_03 |
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| ORD ID | ord-a674ad12d829424a8e074743555aae8c |
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| 出典メモ | uspto-grants-1983_03 |
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