HRID1927273

反应详情

EQUATION

反应方程式

HRID 1927273 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

To a solution of acetonitrile (20 mL) and sodium iodide (2.9 g) was added trimethylsilyl chloride (2.1 g) at room temperature under stirring. The reaction solution thus obtained was cooled to −20° C., and (3-[1,3]dioxolan-2-yl-phenyl)-(5-methyl-thiophen-2-yl)-methanol (1.1 g) described in Manufacturing Example 52-1 and acetonitrile (5 mL) were added thereto under stirring. The reaction solution was returned to room temperature and stirred for 10 minutes. Water was added to the reaction solution, which was then extracted with ethyl acetate. The solvent was evaporated from the organic layer under a reduced pressure, and the residue was purified by silica gel chromatography (heptane:ethyl acetate=2:1) to obtain the titled compound (360 mg).

WORKUP

后处理

  1. customThe reaction solution thus obtained
  2. additionwere added
  3. stirringunder stirring
  4. customwas returned to room temperature
  5. stirringstirred for 10 minutes
  6. extractionwas then extracted with ethyl acetate
  7. customThe solvent was evaporated from the organic layer under a reduced pressure
  8. customthe residue was purified by silica gel chromatography (heptane:ethyl acetate=2:1)