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Diethyl Ether → 2-Butyl-3,5,7,8-tetrahydro-4-oxo-pyrido[4,3-d]pyrimidine-6(4H)-carboxylic acid 2-(trimethylsilyl)ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Pentanimidamide Hydrochloride | HCID 11615174 | — |
| 反応物 | 4-Oxo-1,3-piperidinedicarboxylic acid 3-ethyl 1-[2-(trimethylsilyl)ethyl]ester | HCID 54537175 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Butyl-3,5,7,8-tetrahydro-4-oxo-pyrido[4,3-d]pyrimidine-6(4H)-carboxylic acid 2-(trimethylsilyl)ethyl ester | HCID 136378382 | 32.6% |
反応手順
To a mixture of 2.2 g of 4-oxo-1,3-piperidinedicarboxylic acid 3-ethyl 1-[2-(trimethylsilyl)ethyl]ester and 1.2 g of valeramidine hydrochloride in 15 ml of dry ethyl alcohol is added 7 ml of 1M sodium methoxide in methanol. The resulting mixture is stirred and heated under reflux for 25 minutes. The reaction mixture is allowed to cool, filtered and the solid washed with ethyl alcohol. The combined filtrates are evaporated in vacuo without heat to give an oily solid. Ether and water are added to the residue followed by refrigeration. The resulting crystalline solid is collected, washed with ether and air dried to give 0.8 g of the desired product as a crystalline solid, m.p. 152°-155° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05296480 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-9f3e222c635f4699b0f8cc55846eb83b |
| 出典メモ | uspto-grants-1994_03 |