HRID875411

反应详情

EQUATION

反应方程式

HRID 875411 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of methyl 2,6-dichloro-4-cyanobenzoate (620 mg, 2.6 mmol) in pyridine (5 mL) was treated with anhydrous lithium iodide (1000 mg, 8 mmol). The resulting reaction mixture was stirred at reflux for 1 hour and concentrated under vacuum to remove pyridine. The residue was acidified with hydrochloric acid (2N) under ice-cold condition to adjust the pH between 2 to 3. The precipitated solid was filtered, washed with water and dried to yield 2,6-dichloro-4-cyanobenzoic acid (380 mg, 86%) as a pale brown solid.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. temperatureat reflux for 1 hour
  3. concentrationconcentrated under vacuum
  4. customto remove pyridine
  5. filtrationThe precipitated solid was filtered
  6. washwashed with water
  7. customdried