反应详情

A mixture of 0.110 g (0.307 mmol) of (7RS,9aSR)-7-phenoxymethyl-2-(2-chloropyrimidin-4-yl)-2,3,4,6,7,8,9,9a-octahydro-1H-pyrido[1,2-a]pyrazine (Example 29), 20 mg of 10% Pd/C, and several drops of conc. hydrochloric acid in 30 mL of ethanol were shaken under 50 psi of hydrogen gas at room temperature for 6 h. The mixture was filtered through Celite and the filtrate was evaportated. The residue was basified with conc. ammonium hydroxide, extracted with chloroform, dried (magnesium sulfate), filtered and evaporated. Purification by flash silica gel chromatography with a solvent gradient from 100% chloroform to 95:5 chloroform:methanol gave 0.020 g (20%) of the title compound. mp (—HCl) >265° C. (dec). HRMS calc for C19H24N4O: 324.1945, found: 324.1970.

1. filtrationThe mixture was filtered through Celite
2. extractionextracted with chloroform
3. dry with materialdried (magnesium sulfate)
4. filtrationfiltered
5. customevaporated
6. customPurification by flash silica gel chromatography with a solvent gradient from 100% chloroform to 95:5 chloroform