HRID1863371
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A 42.2 gm. portion of 2,5-dimethyl-4-imidazolemethanol and 44.8 ml. of concentrated nitric acid are mixed. When the initial reaction subsides, the solution is heated on a steam bath for one hour. The reaction mixture is neutralized with concentrated aqueous sodium carbonate, then concentrated under vacuum. After leaching the residue with 150 ml. of hot ethanol several times, the combined organic solutions are concentrated under vacuum. Chromatographing the residual oil on silica gel gives a solid which is recrystallized from iso-propanol-ethyl acetate to give the desired product, m.p. 164.5°-166° C.
WORKUP
后处理
- customWhen the initial reaction subsides
- temperaturethe solution is heated on a steam bath for one hour
- concentrationconcentrated under vacuum
- concentrationof hot ethanol several times, the combined organic solutions are concentrated under vacuum
- customChromatographing the residual oil on silica gel gives a solid which
- customis recrystallized from iso-propanol-ethyl acetate