関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Di-tert-butyl dicarbonate | HCID 90495 | — |
| 反応物 | 3-(4-Carboxy-1-cyclohexyl-butylamino)-5-phenyl-thiophene-2-carboxylic acid methyl ester | HCID 66684832 | — |
| 溶媒 | 1,2-Dioxane | HCID 138570 | — |
| 生成物 | 3-(2-Cyclohexyl-6-oxo-piperidin-1-yl)-5-phenyl-thiophene-2-carboxylic acid methyl ester | HCID 66683946 | 39.3% |
反応手順
To a vial containing a solution of 3-(4-Carboxy-1-cyclohexyl-butylamino)-5-phenyl-thiophene-2-carboxylic acid methyl ester (40 mg, 0.096 mmol, 1.0 equiv) in 1,2-dioxane (1.0 mL) was added pyridine (3.8 mg, 0.048 mmol, 0.5 equiv) and Boc2O (25 mg, 0.166 mmol, 1.2 equiv). The vial was then sealed and heated at 65° C. for 18 hours. The solution was concentrated and the residue was purified by silica gel column chromatography, EtOAc/Heptane 5% to 100% to give product 15 mg (yield 39%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09040690B2 |
|---|
| 出典データセット | uspto-grants-2015_05 |
|---|
| ORD ID | ord-d51df7bce6ca4f8bad3f9a5ca5bb7f2e |
|---|
| 出典メモ | uspto-grants-2015_05 |
|---|