HRID1463981

反应详情

EQUATION

反应方程式

HRID 1463981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 5-amino-4-carboxy-1-(2,2-diethoxyethyl)pyrazole (4 g) in xylene (15.6 ml) was added dropwise 3.4M solution of sodium bis(2-methoxyethoxy)-aluminum hydride in toluene (15.6 ml) at room temperature in an atmosphere of nitrogen. Then the mixture was refluxed for 6 hours, and poured into a mixture of dichloromethane and water. The precipitate was filtered off, and the organic layer was separated and dried over magnesium sulfate. The organic solvent was evaporated in vacuo to give 5-amino-4-methyl-1-[(E)-2-ethoxyvinyl]-pyrazole (598 mg).

WORKUP

后处理

  1. temperatureThen the mixture was refluxed for 6 hours
  2. filtrationThe precipitate was filtered off
  3. customthe organic layer was separated
  4. dry with materialdried over magnesium sulfate
  5. customThe organic solvent was evaporated in vacuo