反应详情

温度

0 °C

In pyridine (600 ml), 31.75 g (86.20 mmol) of the compound from Example 11A were introduced 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 on a frit, after which it was washed with ethanol and ethyl acetate. Subsequently the residue was again stirred with diethyl ether, isolated by filtration with suction and then dried under a 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 on a frit
5. washafter which it was washed with ethanol and ethyl acetate
6. stirringSubsequently the residue was again stirred with diethyl ether
7. customisolated by filtration with suction
8. customdried under a high vacuum