HRID1247830

反应详情

EQUATION

反应方程式

HRID 1247830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-methyl-N5-trityl-1H-pyrazole-4,5-diamine (4 g) in dichloromethane (100 ml) was added tert-butyl 4-{[(2,5-dioxo-1-pyrrolidinyl)oxy]carbonyl}-1-piperidinecarboxylate (4.05 g), and the mixture was refluxed for 72 hours. The reaction mixture was washed successively with water 10% aqueous citric acid solution, water and brine. The extract was dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give tert-butyl 4-({[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]amino}carbonyl)-1-piperidinecarboxylate (1.806 g).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 72 hours
  2. washThe reaction mixture was washed successively with water 10% aqueous citric acid solution, water and brine
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo