反应详情

A mixture of 1.0 g (1.76 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-(6-morpholin-4-yl-4-o-tolyl-pyridin-3-yl)-isobutyramide, 100 mg (0.48 mmol) ruthenium(III)chloride hydrate, 832 mg (3.87 mmol) sodium periodate, 3.5 ml carbon tetrachloride, 3.5 ml acetonitrile and 5.3 ml water was stirred for 4 days at room temperature. Dichloromethane was added, the organic layer was separated, washed with sodium hydrogensulfite solution and filtered over celite. To the filtrate were added 10 ml 1 N potassium hydroxide solution and 20 ml methanol. After heating the mixture for 1 h at 40° C., the solvents were removed in vacuo and the residue was purified by flash-chromatography to give 352 mg (37%) of the title compound as light brown foam.

1. customthe organic layer was separated
2. washwashed with sodium hydrogensulfite solution
3. filtrationfiltered over celite
4. additionTo the filtrate were added 10 ml 1 N potassium hydroxide solution and 20 ml methanol
5. temperatureAfter heating the mixture for 1 h at 40° C.
6. customthe solvents were removed in vacuo
7. customthe residue was purified by flash-chromatography