関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-Bromo-5-trifluoromethylbenzenesulfonamide | HCID 21895504 | — |
| 反応物 | (1S,2R)-4-(2-hydroxy-1-methyl-4-pyridin-3-ylbutoxy)benzeneboronic acid | HCID 54413593 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 57095341 | HCID 57095341 | 75.2% |
反応手順
Prepared according to the method described in Example 12b) from (1S,2R)-4-(2-hydroxy-1-methyl-4-pyridin-3-ylbutoxy)benzeneboronic acid (0.20 g, Example 33), 3-bromo-5-trifluoromethylbenzosulphonamide (0.40 g, Example 74), 2M aqueous sodium carbonate (0.76 ml) and tetrakis(triphenylphosphine)palladium (0) (0.019 g) in ethanol (5 ml) with heating at 90° C. for 4 hours. After work up, the residue was purified by normal-phase HPLC eluting with a gradient of 0-10% ethanol in dichloromethane to give the title compound as a solid (0.24 g). m.p. 57-59° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06300352B1 |
|---|
| 出典データセット | uspto-grants-2001_10 |
|---|
| ORD ID | ord-d294e9131dec49d4928792a670341671 |
|---|
| 出典メモ | uspto-grants-2001_10 |
|---|
