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盐酸 → 3-Fluorophenylacetic acid, 1,1-dimethyl-2-(4-(methylsulfonyl)phenyl)-2-oxo-ethyl ester
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 盐酸 | HCID 313 | — |
| 反应物 | 1-Cyclohexyl-3-(2-morpholinoethyl)carbodiimide metho-p-toluenesulfonate | HCID 17220 | — |
| 反应物 | 3-氟苯乙酸 | HCID 67617 | — |
| 反应物 | 2-Hydroxy-2-methyl-1-(4-(methylsulfonyl)phenyl)propan-1-one | HCID 15428514 | — |
| 催化剂 | 4-二甲氨基吡啶(DMAP) | HCID 14284 | — |
| 溶剂 | 二氯甲烷 | HCID 6344 | — |
| 产物 | 3-Fluorophenylacetic acid, 1,1-dimethyl-2-(4-(methylsulfonyl)phenyl)-2-oxo-ethyl ester | HCID 57265235 | 85.2% |
反应步骤
A mixture of 2-hydroxy-4'-(methylsulfonyl) isobutyrophenone (100 g), 3-fluorophenylacetic acid (83 g), 1-cyclohexyl-3-(2-morpholinoethyl)carbodiimide metho-p-toluenesulfonate (225 g) and DMAP (25 g) in CH2Cl2 (2 L) was mechanically stirred for 17 h at r.t. A solution of 1N HCl (1 L) was then added and the organic phase was separated, washed with a saturated solution of Na2 CO3 (0.4 L) and dried over MgSO4. After concentration, the residue was purified by silica gel chromatography, eluting with 30% EtOAc/hexane to give the title compound as a white solid (133 g).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05840746 |
| 来源数据集 | uspto-grants-1998_11 |
| ORD ID | ord-39c4ea49d34e47ca92197be180b097d3 |
| 来源说明 | uspto-grants-1998_11 |