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温度

0 °C

To an ice-cooled suspension of 1.2 g (7.1 mmol) ruthenium(IV)oxide hydrate in a mixture of 50 ml carbon tetrachloride and 50 ml water were added 9.0 g (42 mmol) sodium periodate. After stirring for 30 min the organic layer was separated and the aqueous layer was extracted twice with 10-ml portions of carbon tetrachloride. The combined organic layers were filtered over celite, cooled to 0° C. and were added slowly to an ice-cooled solution of 2.0 g (3.54 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-(6-morpholin-4-yl-4-o-tolyl-pyridin-3-yl)-isobutyramide in 20 ml carbon tetrachloride. The mixture was stirred for additional 15 min at 0° C., was filtered over celite and was evaporated. The residue was purified by flash-chromatography and gave 704 mg (34%) of the title compound as colourless foam. MS m/e (%): 580 (M+H+, 100).

1. customwas separated
2. extractionthe aqueous layer was extracted twice with 10-ml portions of carbon tetrachloride
3. filtrationThe combined organic layers were filtered over celite
4. additionwere added slowly to an ice-
5. stirringThe mixture was stirred for additional 15 min at 0° C.
6. filtrationwas filtered over celite
7. customwas evaporated
8. customThe residue was purified by flash-chromatography