HRID352442

反应详情

EQUATION

反应方程式

HRID 352442 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 3.41 g of powdered KOH in 110 ml of DMSO was added at 22° C. 6.00 g of {4-[2-(5-methyl-2-phenyl-oxazol-4-yl)-ethoxy]-phenyl}-carbamic acid tert-butyl ester and the suspension was stirred for 25 min. A solution of 7.40 g of 2-bromomethyl-benzoic acid ethyl ester in 10 ml of DMSO was added slowly keeping the temperature at 15-20° C. and stirring was continued at 22° C. for 2.5 h. The dark mixture was partitioned between 500 ml of a saturated aqueous NH4Cl and 200 ml of AcOEt, the organic layer was washed with saturated aqueous NH4Cl and water, dried and evaporated. The residue was purified by chromatography (SiO2, n-hexane/AcOEt 4:1) to give 7.96 g of the title compound as a pale yellow oil. MS: (M+H)+ 557.3.

WORKUP

后处理

  1. additionwas added at 22° C
  2. customat 15-20° C.
  3. customThe dark mixture was partitioned between 500 ml of a saturated aqueous NH4Cl and 200 ml of AcOEt
  4. washthe organic layer was washed with saturated aqueous NH4Cl and water
  5. customdried
  6. customevaporated
  7. customThe residue was purified by chromatography (SiO2, n-hexane/AcOEt 4:1)