HRID1267908

反应详情

EQUATION

反应方程式

HRID 1267908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (3,4-difluorophenyl)-carbamic acid tert-butyl ester (Tetrahedron, (1992), 48(35), 7373) (15.1 g) in tetrahydrofuran (120 ml) at 0° C. was added potassium tert-butoxide (94 ml of a 1.0 M solution in tetrahydrofuran) dropwise. After stirring for 2 hr methyl bromoacetate (9.1 ml) was added dropwise and ice-bath removed and reaction mixture stirred at room temperature overnight. Reaction mixture concentrated under reduced pressure, diluted with ethyl acetate and washed with water and brine, dried (Na2SO4) and concentrated to leave the sub-title compound as a brown oil (18.0 g).

WORKUP

后处理

  1. additionwas added dropwise
  2. customice-bath removed
  3. customreaction mixture
  4. customReaction mixture
  5. concentrationconcentrated under reduced pressure
  6. additiondiluted with ethyl acetate
  7. washwashed with water and brine
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated