反应详情

温度

0 °C

31.75 g (86.20 mmol) of the compound from example 30A were initially charged in pyridine (600 ml) under argon and cooled to 0° C. Then a solution of 6.66 ml (86.20 mmol) of methyl chloroformate in dichloromethane (10 ml) was added dropwise and the mixture was stirred at 0° C. for 1 h. Thereafter, the reaction mixture was brought to RT, concentrated under reduced pressure and co-distilled repeatedly with toluene. The residue was stirred with water/ethanol and then filtered off with suction using a frit, and subsequently washed with ethanol and ethyl acetate. Subsequently, the residue was stirred again with diethyl ether, filtered off with suction and then dried under high vacuum.

1. customwas brought to RT
2. concentrationconcentrated under reduced pressure and co-distilled repeatedly with toluene
3. stirringThe residue was stirred with water/ethanol
4. filtrationfiltered off with suction
5. washsubsequently washed with ethanol and ethyl acetate
6. stirringSubsequently, the residue was stirred again with diethyl ether
7. filtrationfiltered off with suction
8. customdried under high vacuum