HRID1245345

反应详情

EQUATION

反应方程式

HRID 1245345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 3-(3-{[tert-butyl(dimethyl)silyl]oxy}propyl)-dihydropyrimidine-2,4(1H,3H)-dione (100 mg, 0.35 mmol), from this Example step 1, bromobenzene (0.037 mL, 0.35 mmol), tris(dibenzylideneacetone)dipalladium (6.4 mg, 0.01 mmol), Xanthphos (0.0121 g, 0.021 mmol) and Cs2CO3 (0.171 g, 0.52 mmol) were combined in dry dioxane (1 mL) and stirred at 100° C. overnight in a sealed tube. The reaction mixture was partitioned between ethyl acetate and water. Combined organic extracts were washed with water and brine, dried over Na2SO4 and the solvent evaporated in vacuo. The product was purified by preparative TLC using ethyl acetate and hexane (30:70) to give the title compound.

WORKUP

后处理

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. washCombined organic extracts were washed with water and brine
  3. dry with materialdried over Na2SO4
  4. customthe solvent evaporated in vacuo
  5. customThe product was purified by preparative TLC