反应详情

温度

50 °C

A mixture of 125 ml. of acetonitrile, 9.2 g of α,α-bis(p-chlorophenyl)imidazole-2-methanol (prepared according to Example III) and 1.5 g of sodium hydroxide was stirred for one hour. To the--now homogeneous--reaction mixture 500 mg of picric acid and a few crystals of potassium iodide were added and the mixture was heated to 50° C. A solution of 5.2 g of benzyloxymethyl chloride in 50 ml. of acetonitrile was then added dropwise and the reaction mixture was subsequently refluxed for 4 hours. The mixture was cooled and filtered and the filtrate was concentrated under reduced pressure. The residue was suspended in water and the suspension was extracted with diethyl ether. The extract was dried over sodium sulphate and the ether was distilled off. The solid residue obtained was crystallized from isopropyl alcohol. The product was then boiled four times with 75 ml. of petroleum ether (boiling range 60°-80° C.), the petroleum ether being decanted each time, after which it was once again crystallized from isopropyl alcohol. The substance was dried in vacuo for 10 hours at 110° C. 1-[(Benzyloxy)methyl]-α,α-bis(p-chlorophenyl)imidazole-2-methanol was obtained. Melting point 139°-141° C.

1. additionA mixture of 125 ml
2. temperaturethe reaction mixture was subsequently refluxed for 4 hours
3. temperatureThe mixture was cooled
4. filtrationfiltered
5. concentrationthe filtrate was concentrated under reduced pressure
6. extractionthe suspension was extracted with diethyl ether
7. dry with materialThe extract was dried over sodium sulphate
8. distillationthe ether was distilled off
9. customThe solid residue obtained
10. customwas crystallized from isopropyl alcohol
11. customof petroleum ether (boiling range 60°-80° C.), the petroleum ether being decanted each time
12. customafter which it was once again crystallized from isopropyl alcohol
13. customThe substance was dried in vacuo for 10 hours at 110° C