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2-Amino-4,6-dimethoxypyrimidine → Methyl 3 [[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl] aminosulfonyl]-2-thiophenecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-4,6-dimethoxypyrimidine | HCID 118946 | — |
| 反応物 | 2-Thiophenecarboxylic acid, 3-(isocyanatosulfonyl)-, methyl ester | HCID 157296 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 3 [[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl] aminosulfonyl]-2-thiophenecarboxylate | HCID 13390186 | — |
反応手順
To 1.5 g of 2-amino-4,6-dimethoxypyrimidine in 30 ml of anhydrous acetonitrile was added 2.7 g of 2-methoxycarbonyl-3-thiophenesulfonyl isocyanate with stirring at ambient temperature. All of the solid reactant dissolved and after twenty minutes of stirring a precipitate started to form. After two hours the mixture was filtered and the solid which was washed with anhydrous ethyl ether, melted at 191°-193°. The solid showed peaks by nuclear magnetic resonance spectroscopy at 4.0 ppm and 3.8 ppm for the methoxy groups, 6.0 ppm for the H of pyrimidine and 7.6 ppm for the hydrogens on thiophene. The infrared absorption spectrum showed absorption peaks at 1730 and 1700 cm-1 consistent for the two carbonyl peaks in the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04701535 |
| 出典データセット | uspto-grants-1987_10 |
| ORD ID | ord-11f3d1b656764759a62299f35e155c3e |
| 出典メモ | uspto-grants-1987_10 |