HRID580572
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
A mixture of 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.5 g), anhydrous acetonitrile (5 ml), 3-t-butoxycarbonylamino-4-methylpyrrolidine (0.5 g) and DBU (0.25 g) was refluxed for an hour. The reacting mixture was concentrated under reduced pressure, to the resulting residue was added acetonitrile-ether (1:1) to crystallize and the precipitate was collected by filtration. This precipitate was recrystallized from dichloromethane-methanol to give the title compound (0.4 g) as pale yellow powder, mp 213°-215° C.
WORKUP
后处理
- temperaturewas refluxed for an hour
- concentrationThe reacting mixture was concentrated under reduced pressure, to the resulting residue
- additionwas added acetonitrile-ether (1:1)
- customto crystallize
- filtrationthe precipitate was collected by filtration
- customThis precipitate was recrystallized from dichloromethane-methanol