反应详情

温度

5 °C

To a mixture of 7-[(Z)-2-(2-aminothiazol-4-yl)-2-methoxyiminoacetamido]-3-[(E)-1-butenyl]-3-cephem-4-carboxylic acid (130 mg, 0.3 mmole) and K2CO3 (55 mg, 0.4 mmole) in DMF (2.5 ml) was added at 5° C. 1-bromoethyl acetate (67 mg, 0.4 mmole). The mixture was stirred at 5° C. for 1 hour, diluted with ethyl acetate (25 ml), washed successively with water and an aqueous NaCl solution, dried over anhydrous MgSO4 and concentrated in vacuo. The residue was dissolved in chloroform and chromatographed on a silica gel column with 1% methanol in CHCl3. The desired fractions were combined and concentrated in vacuo to yield 77 mg (49%) of the title compound. Estimated purity 90% (by HPLC). Mp. 110°-115° C.

1. additionwas added at 5° C
2. washwashed successively with water
3. dry with materialan aqueous NaCl solution, dried over anhydrous MgSO4
4. concentrationconcentrated in vacuo
5. dissolutionThe residue was dissolved in chloroform
6. customchromatographed on a silica gel column with 1% methanol in CHCl3
7. concentrationconcentrated in vacuo