反应详情

温度

0 °C

To an ice-cooled suspension of 1.2 g (7.12 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.

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