反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To tert-butyl 4-((5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)methyl)-1-piperidinecarboxylate (3.5 g) obtained in Example 85a) was added concentrated hydrochloric acid (10 ml), and mixed for 10 minutes. To the reaction mixture was added ethanol, and the solvent was distilled off under reduced pressure. To the residue was further added ethanol, and the solvent was distilled off under reduced pressure. To the residue was added isopropyl alcohol, and the precipitate was collected by filtration. The precipitate was washed sequentially with isopropyl alcohol and diethyl ether and dried under reduced pressure to obtain 5-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride as a colorless solid (2.5 g, 78%).
WORKUP
后处理
- additionmixed for 10 minutes
- distillationthe solvent was distilled off under reduced pressure
- distillationthe solvent was distilled off under reduced pressure
- additionTo the residue was added isopropyl alcohol
- filtrationthe precipitate was collected by filtration
- washThe precipitate was washed sequentially with isopropyl alcohol and diethyl ether
- customdried under reduced pressure