HRID910034

反应详情

EQUATION

反应方程式

HRID 910034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled (0° C.) solution of (2-acetyl-4-bromophenoxy)acetic acid ethyl ester (2.5 g, 8.3 mmol) in CHCl3 (25 mL) was slowly added bromine (425 uL, 8.3 mmol). After completion the reaction mixture was allowed to stir at room temperature for 1 hour. The mixture was partitioned between CH2Cl2 and brine. The organic phase was washed with brine, dried (MgSO4) and concentrated in vacuo to give the title compound as a white solid (2.97 g, 7.8 mmol, 94%): 1H NMR (CDCl3): δ 1.35 (t, 3H), 4.32 (q, 2H), 4.75 (s, 2H), 4.76 (s, 2H), 6.77 (d, 1H), 7.60 (dd, 1H), 7.97 (s, 1H)

WORKUP

后处理

  1. customThe mixture was partitioned between CH2Cl2 and brine
  2. washThe organic phase was washed with brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo