HRID424826

反应详情

EQUATION

反应方程式

HRID 424826 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-(2-(4-hydroxy-2-methyl-phenyl)-vinyl)-benzoic acid methyl ester (0.09 4 g, 0.351 mmol) and (3-(2,6-dichloro-phenyl)-5-isopropyl-3H-(1,2,3)triazol-4-yl)-methanol (0.100 g, 0.351 mmol) in THF (3 mL) are added triphenylphosphine (0.184 g, 0.702 mmol) and diethyl azodicarboxylate (0.120 g, 0.720 mmol). The reaction is stirred overnight. The reaction is partitioned between ether and water. The organic layer is washed with brine and dried over sodium sulfate. The organic layers are filtered and concentrated. The crude solid is purified via flash chromatography using hexane:ethyl acetate (2:1) as eluent to give 3-(2-(4-(3-(2,6-Dichloro-phenyl)-5-isopropyl-3-H-(1,2,3)triazol-4ylmethyoxy)-2-methyl-phenyl)-vinyl)-benzoic acid methyl ester (0.04 g). ES/MS m/e (35Cl/37Cl) 535.8/538.2 (M+1).

WORKUP

后处理

  1. customThe reaction is partitioned between ether and water
  2. washThe organic layer is washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationThe organic layers are filtered
  5. concentrationconcentrated
  6. customThe crude solid is purified via flash chromatography