HRID1284964
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
PROCEDURE
实验过程
A mixture of 32.12 grams of 2,4-dimethyl-3-nitrophenol, 35.78 grams of methyltosylate and 28.5 grams of anhydrous K2CO3 in 200 ml of acetone is heated to reflux for 12 hours. The reaction mixture is filtered leaving a tan solid. The filtrate is concentrated in vacuo. The concentrated filtrate is taken up in ethyl acetate and washed with 10% aqueous sodium hydroxide solution and saturated aqueous sodium chloride. The remaining ethyl acetate layer is dried, filtered and concentrated in vacuo to give a dark oil which is distilled (T=80°-87° C./50μ) to give 30.95 grams of a yellow solid which is recrystallized from absolute ethanol, M.P. 53°-55° C.
WORKUP
后处理
- temperatureis heated
- temperatureto reflux for 12 hours
- filtrationThe reaction mixture is filtered
- customleaving a tan solid
- concentrationThe filtrate is concentrated in vacuo
- washwashed with 10% aqueous sodium hydroxide solution and saturated aqueous sodium chloride
- dry with materialThe remaining ethyl acetate layer is dried
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a dark oil which
- distillationis distilled (T=80°-87° C./50μ)