HRID414020

反应详情

EQUATION

反应方程式

HRID 414020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl iodide (32.3 ml, 0.519 mol), potassium carbonate (14.4 g, 0.104 mol), and product of Step 2 (25.0 g, 0.086, 5 mol) in acetone (100 ml) was refluxed for 18 hours and concentrated. The residue was dissolved in ether and washed with water. The ether layer was worked up as usual. The crude product, a yellow solid (27.25 g), was recrystallized (chloroform petroleum ether) to afford white rods (22.95 g), yield--88%; mp 101°-103° C.

WORKUP

后处理

  1. temperaturewas refluxed for 18 hours
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ether
  4. washwashed with water
  5. customThe crude product, a yellow solid (27.25 g), was recrystallized (chloroform petroleum ether)
  6. customto afford white rods (22.95 g)
  7. customyield--88%