HRID1589182

反应详情

EQUATION

反应方程式

HRID 1589182 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.54 g. of 4-fluorophenylacetic acid, 1.62 g. of 1,1'-carbonyldiimidazole and 30 ml. of tetrahydrofuran was stirred for 2 hours, then 1.98 g. of 1H-imidazole-1-propanamine dihydrochloride was added. Stirring was continued at room temperature for an additional 18 hours, then at reflux temperature for 5 hours, 5 ml. of water was added, the mixture was heated for 30 minutes and then concentrated to remove the volatile material. The residue was diluted with methylene chloride and 25 ml. of 1N sodium hydroxide and the layers separated. The organic layer was washed with water, dried over magnesium sulfate and concentrated, giving the desired product as a viscous oil.

WORKUP

后处理

  1. additionA mixture of 1.54 g
  2. temperatureat reflux temperature for 5 hours
  3. temperaturethe mixture was heated for 30 minutes
  4. concentrationconcentrated
  5. customto remove the volatile material
  6. additionThe residue was diluted with methylene chloride and 25 ml
  7. customof 1N sodium hydroxide and the layers separated
  8. washThe organic layer was washed with water
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated