HRID1161504

反应详情

EQUATION

反应方程式

HRID 1161504 的结构方程式

PROCEDURE

实验过程

After adding 25 ml of trifluoroacetic acid to a solution of 3.30 g of 3-(N′-t-butoxycarbonylhydrazino)-1H-pyrazole-4-carboxylic acid ethyl ester in 50 ml of dichloromethane, the mixture was stirred for 2 hours at room temperature. Next, 100 ml of toluene was added and the solvent was removed under reduced pressure. The residue was dissolved in a small amount of methanol, and after adding a 4N solution containing hydrochloric acid in ethyl acetate until the solution reached acidic, the solvent was removed under reduced pressure. The residue was treated with 50 ml of t-butyl methyl ether, and the solid was filtered off and dried under reduced pressure to give the title compound (3.30 g) as a white solid.

WORKUP

后处理

  1. customthe solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in a small amount of methanol
  3. additionafter adding a 4N solution
  4. additioncontaining hydrochloric acid in ethyl acetate until the solution
  5. customthe solvent was removed under reduced pressure
  6. additionThe residue was treated with 50 ml of t-butyl methyl ether
  7. filtrationthe solid was filtered off
  8. customdried under reduced pressure