HRID547979

反应详情

EQUATION

反应方程式

HRID 547979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.07 g of 1-methyl-2-phenyl-1H-indole, 1.32 g of 1,1-dimethoxy-3-butanone and 12 mL of acetic acid were mixed, then, 313 mg of 35 wt % hydrochloric acid was added into the mixture at room temperature, the added mixture was stirred for about 14 hours at the same temperature to cause a reaction. At a time point about 10 minutes after starting of stirring and reaction, blue solid precipitated to render stirring difficult. Therefore, 8 mL of acetic acid was added. After completion of the reaction, 60 mL of water was added dropwise, and the precipitated crystals were filtrated. The crystals were washed with 10 vol % methanol/water, then, dried to obtain 2.44 g of trans-4-[1-methyl-2-phenyl-1H-indol-3-yl]-3-buten-2-one (blue green solid). Yield: 89%.

WORKUP

后处理

  1. customa reaction
  2. customAt a time point about 10 minutes
  3. stirringof stirring
  4. customreaction, blue solid
  5. customprecipitated
  6. stirringto render stirring difficult
  7. additionTherefore, 8 mL of acetic acid was added
  8. customAfter completion of the reaction, 60 mL of water
  9. additionwas added dropwise
  10. filtrationthe precipitated crystals were filtrated
  11. washThe crystals were washed with 10 vol % methanol/water
  12. customdried