反应详情

A mixture of 1-(4-chlorobutyl)-2-ethyl-2H-pyrazolo[3,4-c]quinolin-4-amine (3 g, prepared as described in Example 19), platinum (IV) oxide (3 g), and trifluoroacetic acid (50 mL) was placed under hydrogen pressure (50 psi, 3.4×105 Pa) on a Parr shaker for 2 days. The reaction mixture was filtered through a layer of CELITE filter agent and the filter cake was rinsed with dichloromethane. The filtrate was concentrated under reduced pressure. The residue was made basic (p H 14) by the addition of 50% sodium hydroxide and then extracted with chloroform. The extract was dried over sodium sulfate and then purified by chromatography on a HORIZON HPFC system (eluting with chloroforn/CMA in a gradient from 100:0 to 70:30) to provide 1.75 g of 1-(4-chlorobutyl)-2-ethyl-6,7,8,9-tetrahydro-2H-pyrazolo[3,4-c]quinolin-4-amine as a light yellow solid.

1. customfor 2 days
2. filtrationThe reaction mixture was filtered through a layer of CELITE filter agent
3. washthe filter cake was rinsed with dichloromethane
4. concentrationThe filtrate was concentrated under reduced pressure
5. additionby the addition of 50% sodium hydroxide
6. extractionextracted with chloroform
7. dry with materialThe extract was dried over sodium sulfate
8. custompurified by chromatography on a HORIZON HPFC system (
9. washeluting with chloroforn/CMA in a gradient from 100:0 to 70:30)