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Sodium Methoxide → 2-Butyl-6-(2,2-dimethyl-1-oxopropyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-4(3H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Pentanimidamide Hydrochloride | HCID 11615174 | — |
| 反応物 | Ethyl 1-(2,2-dimethyl-1-oxopropyl)-4-oxo-3-piperidinecarboxylate | HCID 19102683 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Butyl-6-(2,2-dimethyl-1-oxopropyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-4(3H)-one | HCID 135674970 | 67.4% |
反応手順
A mixture of 1.3 g of ethyl 1-(2,2-dimethyl-1-oxopropyl)-4-oxo-3-piperidinecarboxylate and 0.75 g of valeramidine hydrochloride in 10 ml of anhydrous ethyl alcohol is treated with 5.3 ml of a 1M solution of sodium methoxide in methanol. The resulting mixture is stirred and heated at reflux for one hour. The reaction mixture is allowed to cool over 30 minutes then filtered. The filtrate is evaporated to a gummy residue and stirred with 40 ml of ether for 30 minutes, filtered and the cake washed with ether. The cake is dried at 56° C. under vacuum to afford 1.0 g of the desired product as a colorless solid, m.p. 167°-172° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05281602 |
| 出典データセット | uspto-grants-1994_01 |
| ORD ID | ord-b184e56a4caf4599a1d7f0c6a1db0177 |
| 出典メモ | uspto-grants-1994_01 |