反应详情

温度

80 °C

2.65 g of teicoplanin complex (i.e. the antibiotic complex containing teichomycin factors A1, A2 and A3, as obtained by fermentation of strain ATCC 31121 according to U.S. Pat. No. 4,239,751), is dissolved with stirring into 180 ml of acetic acid. To this solution 20 ml of 37% (w/v) HCl are added and the mixture is heated at 80° C. for one hour (the reaction time has been determined according to previous experiments where the reaction was followed by HPLC). After cooling to room temperature, the reaction mixture is poured into 1 liter of ice-cooled ethyl ether. The obtained precipitate is collected by filtration, washed with ethyl ether and then dissolved in 60 ml of a mixture of methanol and 0.1 N HCl 3:2 (v/v). To the resulting solution, 600 ml of a mixture of water/ethyl acetate/n-butanol 4:5:1 (v/v/v) are added and the pH is adjusted to 8.5 by adding 1 N NaOH. The organic layer is then discarded and the aqueous phase chromatographed through a column prepared with 270 g of silanized silica gel as described in the last part of Example 4. Yield 750 g of substantially pure deglucoteicoplanin.

1. customas obtained by fermentation of strain ATCC 31121 according to U.S
2. dissolution4,239,751), is dissolved
3. temperatureAfter cooling to room temperature
4. filtrationThe obtained precipitate is collected by filtration
5. washwashed with ethyl ether
6. dissolutiondissolved in 60 ml of a mixture of methanol and 0.1 N HCl 3:2 (v/v)
7. additionTo the resulting solution, 600 ml of a mixture of water/ethyl acetate/n-butanol 4:5:1 (v/v/v) are added
8. additionby adding 1 N NaOH
9. customthe aqueous phase chromatographed through a column
10. customprepared with 270 g of silanized silica gel