HRID1775376
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
tert-Butyl 4-(4-ethoxy-6-methyl-2-pyridyl)piperazine-1-carboxylate (141 mg, 0.44 mmol) was dissolved in a mixture of DCM (5 ml) and trifluorocrotonic acid (5 ml) and left standing at room temperature for two hours. The mixture was concentrated under reduced pressure, the residue was dissolved in THF, evaporated again, dissolved again in THF. Hydrochloric acid (4N in dioxane) was added to precipitate the product, which was collected by filtration, washed with diethylether and dried under reduced pressure to give 115 mg (quantitative) MS (multi-mode) m/z=222.2 [M+H]+.
WORKUP
后处理
- waitleft
- concentrationThe mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in THF
- customevaporated again
- dissolutiondissolved again in THF
- additionHydrochloric acid (4N in dioxane) was added
- customto precipitate the product, which
- filtrationwas collected by filtration
- washwashed with diethylether
- customdried under reduced pressure
- customto give 115 mg (quantitative)