HRID1529

反应详情

EQUATION

反应方程式

HRID 1529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium carbonate (1.95 g, 14.2 mMol) was added to a solution of (R)-2-(4-hydroxyphenyl)-1-methylethylcarbamic acid, t-butyl ester (2.96 g, 11.8 mMol) in acetone (50 ml) at room temperature under argon. Methyl bromoacetate (1.81 g, 11.8 mMol) was added dropwise and the reaction mixture was heated at reflux for 3 hours. The solvent was removed under reduced pressure and the residue was taken into ethyl acetate and washed with water (2×30 ml). The organic extracts were dried with sodium sulfate and the solvent evaporated in vacuo. The crude product was purified by chromatography on Kieselgel 60 (eluting with 20% ethyl acetate in pentane) to give the title compound as an oil.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 3 hours
  3. customThe solvent was removed under reduced pressure
  4. washwashed with water (2×30 ml)
  5. dry with materialThe organic extracts were dried with sodium sulfate
  6. customthe solvent evaporated in vacuo
  7. customThe crude product was purified by chromatography on Kieselgel 60 (eluting with 20% ethyl acetate in pentane)