反应详情

(1-Pyrryl)acetic is added to water, the pH of which is adjusted to about 6.5 by the addition of sodium bicarbonate. This solution is cooled in an ice bath and to it is added one equivalent of 3-[[(5 methyl - 1, 3, 4-thiadiazol-2-yl) thio]methyl]-7-amino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid (7-ATDCA) followed by N, N'-dicyclohexylcarbodiimide in cold dioxane. The mole ratio of (1-pyrryl) acetic acid/7-ATDCA/carbodiimide is 3/1/1. After standing overnight at ice bath temperature, the reaction mixture is filtered to remove solids. The filtrate is evaporated to dryness, the solids taken up in ethyl acetate, dried over magnesium sulfate and filtered. The ethyl acetate solution is concentrated and then treated with hexane. The title compound precipitates from solution is filtered and dried. EXAMPLE 6

1. temperatureThis solution is cooled in an ice bath and to it
2. filtrationtemperature, the reaction mixture is filtered
3. customto remove solids
4. customThe filtrate is evaporated to dryness
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationThe ethyl acetate solution is concentrated
8. additiontreated with hexane
9. customThe title compound precipitates from solution
10. filtrationis filtered
11. customdried