HRID1046009

反应详情

EQUATION

反应方程式

HRID 1046009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-chloro-5-fluorophenol (1.50 g, 10.24 mmol), 3-bromo-4-chloropyridine (1.50 g, 7.79 mmol) and DBU (1.50 g, 9.85 mmol) were heated at 130° C. in NMP (10 mL) for 15 hours. The reaction mixture was cooled and partitioned between water (100 mL) and MTBE (100 mL). The organic layer was separated, washed with dilute aq NaOH and brine, dried (MgSO4) and concentrated in vacuo to provide 3-bromo-4-(2-chloro-5-fluorophenoxy)pyridine (1.98 g, 84% yield) as brownish oil suitable for use in the next reaction. MS (ESI) m/z: 303.9 (M+H+).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. custompartitioned between water (100 mL) and MTBE (100 mL)
  3. customThe organic layer was separated
  4. washwashed with dilute aq NaOH and brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo