反应详情

温度

-25 °C

To a suspension of 14.9 g of penicillin-G-potassium (= 40 mmols) in 60 ml of absolute methylene chloride 10 ml of N,N-dimethylaniline and 8.42 g (= 40 mmols) of methyl-n-octylphosphinic acid chloride were added successively while stirring. After an hour at 0°C the reaction mixture was cooled to -25°C and 9.0 g (= 43 mmols) of phosphorus pentachloride were introduced. After an hour at -25°C, 60 ml of n-butanol and 2 ml of N,N-dimethylaniline were introduced and by after-stirring for an hour at -25°C the iminoether was formed. Then, hydrolysis followed in the manner described in Example 1. 7.47 g (= 88.5 % of the theory) of 6-aminopenicillanic acid having a melting point of 195°C (decomposition) were isolated in the form of colorless crystals, the identity of which was examined in an analogous manner as described in Example 1.

1. additionwere added successively
2. waitAfter an hour at -25°C
3. customwas formed
4. customThen, hydrolysis