HRID1785377

反应详情

EQUATION

反应方程式

HRID 1785377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a reactor were fed 2.4 g (12.2 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone, 1.7 g (9.98 m moles) of 2-ethylphenylhydrazine hydrochloride, 1.4 g (10.2 m moles) of zinc chloride and 10 ml of toluene, followed by refluxing for 2 hours with heating. After the completion of the reaction, the reaction mixture was cooled to room temperature. Thereto were added water and ethyl acetate and phase separation was made. The ethyl acetate layer was concentrated. The concentrate was subjected to silica gel column chromatography separation (developing solvent: n-hexane/ethyl acetate) to obtain 2.38 g (8.01 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2-methyl-7-ethylindole.

WORKUP

后处理

  1. customInto a reactor were fed
  2. temperatureby refluxing for 2 hours
  3. temperaturewith heating
  4. customAfter the completion of the reaction
  5. additionThereto were added
  6. customwater and ethyl acetate and phase separation
  7. concentrationThe ethyl acetate layer was concentrated
  8. customThe concentrate was subjected to silica gel column chromatography separation (developing solvent: n-hexane/ethyl acetate)