SU530646A3 - The method of obtaining derivatives of 7-monochloroacetamido-3-deacetoxycephalosporanic acid - Google Patents

Claims (1)

(54) METHOD | 1TORACTIONS OF 7-MONOCHLORACETAMIDO DERIVATIVES-. --3-DEATACETOXYCEPHALOSPORIC ACID J., 5 ml of acetic acid and 1.16 g of ZINC powder are stirred for 2 hours at 20 ° C. The flocne filtering mixture was poured into ice water and the pH was adjusted to 2 by adding 1 and. hydrochloric acid when mixed. The solid is filtered off, washed 5 times with 50 ml of water and diluted with 1OO ml of ethyl acetate. This organic phase is washed 2 times with 1bb ml of V - t - -.j - ,,% A. ъ. J. h-v-iv4 "A s, dried over sodium sulfate, filtered M and distilled to dryness under reduced pressure (12 mm Hg) at 30 ° C. A solid colorless solid of 68OmA is obtained, which is dissolved in 10 ml of methylene chloride. The resulting solution is chromatographed on a column of 50 g; silica gel {O ,, 2O ml, pH neutral; column diameter 1.4 cm, height 40 cm). Elute one after another 100 ml of methylene chloride, 25 O ml of a mixture of methylene chloride - e-acetate (98: 2 by volume) and 750 ml of methylene chloride - ethyl acetate (96: 4 by volume), 50 fractions ml. Combine the fractions from the 8th to the 2nd and concentrate them under reduced pressure (12 mm Hg) at ZO C. The residue is thoroughly dissolved in 10 ml of diethyl ether. After filtration and sushi, 420 mg of 7 | -; methoxybenzyl fir 7-chloroacetamido-4-toxoacephalospanoic acid are obtained, b.p. 166 ° C. Claim 1. Method for producing T-mo-p derivatives of ochlorac © tamido-3-deacetoxycephalospores with najfi / 4v tj Mt3: xam Sound of formulas of formula 1 benzyl or p methoxybenzyl; and with the fact that there are compounds of formula II, Ct6 fcONH rY // - to where R has the above values; Processed with zinc in acetic acid.