反应详情

温度

-30 °C

A mixture of benzhydryl 7-(2-phenylacetamido)-3-[2-(2-propynyl)-2H-tetrazol-5-yl]thiomethyl-3-cephem-4-carboxylate-1-oxide (16.0 g) and dry N,N-dimethylformamide (160 ml) was cooled to -30° C. and thereto was added phosphorus trichloride (6.7 g). The resulting solution was stirred for 50 minutes at -30° C. The reaction mixture was allowed to warm to ambient temperature, added to water (200 ml) and then extracted with ethyl acetate (×3). The extracts were combined, washed successively with a saturated aqueous solution of sodium bicarbonate (×3) and water (×3), dried over magnesium sulfate, treated with activated charcoal and then evaporated. The residue was pulverized in a mixture of isopropyl ether and n-hexane, collected by filtration, washed with n-hexane and then dried to give benzhydryl 7-(2-phenylacetamido)-3-[2-(2-propynyl)-2H-tetrazol-5-yl]thiomethyl-3-cephem-4-carboxylate (14.33 g).

1. temperatureto warm to ambient temperature
2. extractionextracted with ethyl acetate (×3)
3. washwashed successively with a saturated aqueous solution of sodium bicarbonate (×3) and water (×3)
4. dry with materialdried over magnesium sulfate
5. additiontreated with activated charcoal
6. customevaporated
7. additionThe residue was pulverized in a mixture of isopropyl ether and n-hexane
8. filtrationcollected by filtration
9. washwashed with n-hexane
10. customdried