関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 5-Chloro-thiophene-2-carboxylic acid (2-{(1-isopropyl-piperidin-4-yl)-[3-(tetrahydro-pyran-2-yloxy)-propyl]-sulfamoyl}-ethyl)-amide | HCID 66624965 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Fumaric Acid | HCID 444972 | — |
| 生成物 | Fumarate | HCID 5460307 | — |
| 生成物 | 5-Chloro-thiophene-2-carboxylic acid {2-[(3-hydroxy-propyl)-(1-isopropyl-piperidin-4-yl)-sulfamoyl]-ethyl}-amide | HCID 66624819 | — |
反応手順
220 mg (0.38 mmol) 5-Chloro-thiophene-2-carboxylic acid (2-{(1-isopropyl-piperidin-4-yl)-[3-(tetrahydro-pyran-2-yloxy)-propyl]-sulfamoyl}-ethyl)-amide were dissolved in a mixture of 4 ml THF, 8 ml conc. acetic acid and 2 ml water. The resulting mixture was stirred for 8 h at 60° C., concentrated under reduced pressure and purified by preparative RP-HPLC (CH3CN/H2O gradient+0.1% TFA). The product was taken up in dichloromethane and treated with a saturated NaHCO3-solution. After phase separation the organic phase was concentrated and the resulting residue was dissolved in water containing 1 equiv. of fumaric acid. Lyophilisation gave the title compound as its fumarate in form of a colorless amorphous material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08088925B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-4e5d5f52a9e54776b1dde07c9ebdf502 |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|
