反应详情

When 0.2 ml of 69% w/v aqueous nitric acid was added to a solution of 865 mg of trans-1-[6-(2,6-dichlorobenzyloxy)tetrahydropyran-2-ylmethyl]imidazole in 10 ml of diethyl ether, the solution became turbid and an oily layer separated. After decanting off the ethereal layer, more diethyl ether was added to the residue to aid crystallization and the precipitated crystals were filtered, to give 846 g of the title product. Further recrystallization of these crystals from a mixture of acetone and ethyl acetate gave the title product in the form of colourless crystals melting at 117° C.

1. customan oily layer separated
2. customAfter decanting off the ethereal layer, more diethyl ether
3. additionwas added to the residue
4. customcrystallization
5. filtrationthe precipitated crystals were filtered