HRID916826

反应详情

EQUATION

反应方程式

HRID 916826 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution of [4-(2-bromoethyl)phenoxy](tert-butyl)dimethylsilane (479 mg) in DMF (20 ml) under nitrogen was treated with (1R)-2-amino-1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)ethanol (678 mg) and the mixture was stirred at 20° C. for 9.5 h. Phosphate buffer solution (pH 6.5) was added and the mixture was extracted with EtOAc. The extract was washed with water and dried (Na2SO4). Solvent evaporation in vacuo gave a residue which was purified by SPE (10 g). Elution with DCM then DCM-EtOH-0.880 ammonia solution (300:8:1) then (150:8:1) gave the title compound (991 mg). LCMS RT=3.13 min.

WORKUP

后处理

  1. extractionthe mixture was extracted with EtOAc
  2. washThe extract was washed with water
  3. dry with materialdried (Na2SO4)
  4. customSolvent evaporation in vacuo
  5. customgave a residue which
  6. customwas purified by SPE (10 g)
  7. washElution with DCM