HRID453545

反应详情

EQUATION

反应方程式

HRID 453545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a stirred solution of methyl 4-(4-(2-tert-butoxy-2-oxoethyl)-2-((N-methylmethylsulfonamido)methyl)phenoxy)benzoate (370 mg, 0.797 mmol) in dioxane (8 ml) was added a solution of LiOH monohydrate (43.5 mg, 1.04 mmol) in water (2 ml) (0.1M solution 4:1 dioxane/water). The reaction was stirred for 5 hours, then diluted with dichloromethane and 2N HCl. The aqueous phase was extracted with dichloromethane and the combined organic layers were washed with brine and dried over MgSO4. The crude product was purified by silica gel chromatography to give 4-(4-(2-tert-butoxy-2-oxoethyl)-2-((N-methylmethylsulfonamido)methyl)phenoxy)benzoic acid (0.253 g).

WORKUP

后处理

  1. extractionThe aqueous phase was extracted with dichloromethane
  2. washthe combined organic layers were washed with brine
  3. dry with materialdried over MgSO4
  4. customThe crude product was purified by silica gel chromatography