反应详情

温度

65 °C

A solution of 1.5 g (4.6 mmol) (RS)-6-(4-methyl-piperazin-1-yl)-4-o-tolyl-4,5-dihydro-pyridine-3-carboxylic acid methylamide in 15 ml CHCl3 was treated with 2.3 g (23.0 mmol) MnO2. The black suspension was heated to 65° C., stirred for 3 h at 65° C. and treated again with 2.3 g (23.0 mmol) MnO2, stirred for 3 h and added an other 0.9 g (9.2 mmol) MnO2. The reaction mixture was stirred for 10.5 h at 65° C., treated with 0.9 g (9.2 mmol) MnO2, stirred for 1 h at 65° C. and cooled to r.t. After filtration of the MnO2 the solvent was removed under reduced pressure and the residue purified by chromatography over silica gel (CHCl3: MeOH =4:1) to yield 1.24 g (83.2%) product as beige foam.

1. stirringstirred for 3 h
2. stirringThe reaction mixture was stirred for 10.5 h at 65° C.
3. stirringstirred for 1 h at 65° C.
4. temperaturecooled to r.t
5. filtrationAfter filtration of the MnO2 the solvent
6. customwas removed under reduced pressure
7. customthe residue purified by chromatography over silica gel (CHCl3: MeOH =4:1)