HRID2182140

反应详情

EQUATION

反应方程式

HRID 2182140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,6-dichloropyrazine (400 mg, 0.671 mmol), 3-hydroxymethyl-benzonitrile (428 mg, 0.805 mmol), KOH (181 mg, 0.805 mmol) and 18-crown-6 (28 mg, 0.027 mmol) in toluene (10 mL) was stirred at reflux for 6 h and concentrated in vacuo. The residue was partitioned between H2O and ethyl acetate. The aqueous phase was separated and extracted with ethyl acetate twice. The combined organic extracts were washed with water and brine, dried and concentrated in vacuo. The crude product I-3f (667.2 mg) was used for next step without further purification.

WORKUP

后处理

  1. temperatureat reflux for 6 h
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between H2O and ethyl acetate
  4. customThe aqueous phase was separated
  5. extractionextracted with ethyl acetate twice
  6. washThe combined organic extracts were washed with water and brine
  7. customdried
  8. concentrationconcentrated in vacuo
  9. customThe crude product I-3f (667.2 mg) was used for next step without further purification