反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Under a nitrogen atmosphere, a mixture of 2-(4-aminobutyl)-7-benzyloxy-1-(2-phenoxyethyl)-1H-imidazo[4,5-c]quinolin-4-amine (0.40 g, 0.83 mmol) and pyridine (10 mL) was cooled to 0° C., and phenyl isocyanate (91 μL, 0.84 mmol) was added. The reaction was stirred for one hour and additional phenyl isocyanate (10 μL) was added. The reaction was stirred for one hour and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluting with 95:5-chloroform:methanol), recrystallized from toluene, and dried in a vacuum oven to provide 150 mg of TV-{4-[4-amino-7-benzyloxy-1-(2-phenoxyethyl)-1H-imidazo[4,5-c]quinolin-2-yl]butyl}-N′-phenylurea as a white crystalline solid, mp 186.3-186.9° C.
WORKUP
后处理
- stirringThe reaction was stirred for one hour
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography on silica gel (eluting with 95:5-chloroform:methanol)
- customrecrystallized from toluene
- customdried in a vacuum oven