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Dimethylformamide dimethyl acetal → (E)-ethyl 4-(2-(dimethylamino)vinyl)-2-(methylthio)pyrimidine-5-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | Ethyl-2-methylthio-4-methyl-5-pyrimidine carboxylate | HCID 188208 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (E)-ethyl 4-(2-(dimethylamino)vinyl)-2-(methylthio)pyrimidine-5-carboxylate | HCID 86657908 | 62% |
反応手順
4-Methyl-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester 3 (18.0 g, 84.8 mmol) was dissolved in DMF (50 mL), N,N-Dimethylformamidedimethylacetal (22.5 mL, 170 mmol) and stirred at reflux for 3 hours. Then mixture was concentrated, the residue was dissolved in TCM, washed with water, dried, filtered, and concentrated. The product was purified by crystallization from ether to yield in a colorless solid (14.0 g, 52.5 mmol, 62%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530650B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-dc974b9b448b4f40ae01977f5f513159 |
| 出典メモ | uspto-grants-2013_09 |