反应详情

7.65 ml (104.8 mmol) of thionyl chloride were added dropwise with ice cooling to a suspension of 15 g (52.4 mmol) of 4-(3-(2-methylphenyl)ureido)-3-methoxybenzyl alcohol in 300 ml of dichloromethane. The reaction mixture was subsequently stirred at room temperature for 3 hours, allowed to stand overnight and then poured onto 1000 ml of n-heptane. The heptane was decanted off from the deposited oil, the residue was again suspended with n-heptane and the heptane was decanted off. This process was repeated a further two times. The residue was then dissolved in dichloromethane and poured into 800 ml of ice-cold diisopropyl ether. It was subsequently stirred with ice cooling for 2 hours, and the product was filtered off with suction and washed with diisopropyl ether. After drying over phosphorus pentoxide, 12 g (75%) of the title compound were obtained.

1. waitto stand overnight
2. customThe heptane was decanted off from the deposited oil
3. customthe heptane was decanted off
4. dissolutionThe residue was then dissolved in dichloromethane
5. additionpoured into 800 ml of ice-cold diisopropyl ether
6. stirringIt was subsequently stirred with ice cooling for 2 hours
7. filtrationthe product was filtered off with suction
8. washwashed with diisopropyl ether
9. dry with materialAfter drying over phosphorus pentoxide