反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customthe solvent was removed under reduced pressure
- dissolutionThe residue was dissolved in a small amount of methanol
- additionafter adding a 4N solution
- additioncontaining hydrochloric acid in ethyl acetate until the solution
- customthe solvent was removed under reduced pressure
- additionThe residue was treated with 50 ml of t-butyl methyl ether
- filtrationthe solid was filtered off
- customdried under reduced pressure