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. MS m/e (%): 540 (M+H+, 100).

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