HRID2416680

反应详情

EQUATION

反应方程式

HRID 2416680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-bromo-3-bromomethylanisole (24 g, 86 mmol) and potassium di-tert-butyl iminodicarboxylate (24 g, 94 mmol) in dimethylformamide (200 mL) was stirred under argon at room temperature for 18 hr. The reaction was then concentrated under vacuum and the residue was partitioned between ethyl acetate and water. The organic phase was washed with water and brine, dried(MgSO4), and concentrated. The residue was recrystallized from hexane to give the title compound (15 g, 42%) as a white solid: 1H NMR (CDCl3) δ 7.40 (d, J=8.6 Hz, 1 H), 6.68 (m, 2 H), 4.81(s, 2 H), 3.74 (s, 3 H) 1.44 (s, 18 H).

WORKUP

后处理

  1. concentrationThe reaction was then concentrated under vacuum
  2. customthe residue was partitioned between ethyl acetate and water
  3. washThe organic phase was washed with water and brine, dried(MgSO4)
  4. concentrationconcentrated
  5. customThe residue was recrystallized from hexane