関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4,6-Dichloro-2-methylpyrimidine | HCID 234997 | — |
| 反応物 | 2-Amino-4-methyl-thiazole-5-carboxylic acid | HCID 832243 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | Methyl 2-(6-chloro-2-methylpyrimidin-4-yl-amino)thiazol-5-carboxylic acid | HCID 118319269 | 87.3% |
反応手順
In a reaction flask, 49.49 g 4,6-dichloro-2-methylpyrimidine (0.303 mol), 40.00 g methyl 2-aminothiazol-5-carboxylic acid (0.253 mol), and 200 ml N,N-dimethylacetamide were charged, the temperature was brought to −5° C. and 18.20 g sodium hydride (0.455 mol) in 90 ml tetrahydrofuran were added dropwise and the reaction mixture was kept under these conditions for about three hours. At the end of the reaction, 250 ml of a solution of hydrochloric acid 2N were added, the temperature was brought to the room value, the formed solid was filtered and washed with water (4×200 ml) and dried in oven under vacuum at a temperature of 55° C. for about eight hours, to give 62.89 g methyl 2-(6-chloro-2-methylpyrimidin-4-yl-amino)thiazol-5-carboxylic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09115124B1 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-c6b4fa359e61427087f2bde4f7340faf |
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| 出典メモ | uspto-grants-2015_08 |
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