HRID1284964

反应详情

EQUATION

反应方程式

HRID 1284964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureis heated
  2. temperatureto reflux for 12 hours
  3. filtrationThe reaction mixture is filtered
  4. customleaving a tan solid
  5. concentrationThe filtrate is concentrated in vacuo
  6. washwashed with 10% aqueous sodium hydroxide solution and saturated aqueous sodium chloride
  7. dry with materialThe remaining ethyl acetate layer is dried
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customto give a dark oil which
  11. distillationis distilled (T=80°-87° C./50μ)