関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Bromo-5-piperidin-1-yl-pyrazine-2-carboxylic acid methyl ester | HCID 86619522 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 6-Isopropoxy-5-piperidin-1-yl-pyrazine-2-carboxylic acid | HCID 68569451 | 21.3% |
反応手順
A mixture of 0.212 g (0.707 mmol) 6-bromo-5-piperidin-1-yl-pyrazine-2-carboxylic acid methyl ester, 0.006 g (0.778 mmol) isopropanol and 0.034 g (0.778 mmol) NaH (55% dispersion in oil) in 1.7 mL dioxane was heated to 60° C. for 16 h. Water and 5N KOH was added and the mixture was heated to 50° C. for 4 h. Formic acid and DMF was added and the mixture was subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and formic acid. The product fractions were combined and evaporated to yield 0.04 g (21%) of the title compound. m/z (ES+): 266.4 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07691863B2 |
|---|
| 出典データセット | uspto-grants-2010_04 |
|---|
| ORD ID | ord-3fb8e08a922a48e4bc637cbb983a6acc |
|---|
| 出典メモ | uspto-grants-2010_04 |
|---|
