HRID1689780

反应详情

EQUATION

反应方程式

HRID 1689780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trans-5-cyclopropyl-3-(2,6-dichloro-phenyl)-4-{4-[4-(4-methoxy-benzyloxy)-phenyl]-cyclohexyloxymethyl}isoxazole (1.33 mmol, 770.00 mg) in dichloromethane (17 mL) is treated at room temperature with methoxybenzene (13.3 mmol, 1.45 mL) and trifluoroacetic acid (8.5 mL). The solution is stirred for 2 h and concentrated under reduced pressure. The residue is co-evaporated with CCl4 (2×) and triturated with hexanes. The crude product is supported on silica gel and purified by flash chromatography (120 g silica) eluting with a gradient of 20-50% EtOAc in hexane to give the title compound (544 mg, 89%) as a white solid. MS m/z 458.0 (M+1).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customtriturated with hexanes
  3. custompurified by flash chromatography (120 g silica)
  4. washeluting with a gradient of 20-50% EtOAc in hexane