反应 #80271

ord-b85621a70dcc4cf1a64757f4dd2df935

反应条件

温度
70°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    其他was returned to room temperature
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤The organic layer was washed with water
  5. 5
    干燥dried over anhydrous sodium sulfate
  6. 6
    浓缩Then, it was concentrated under reduced pressure
  7. 7
    其他the oily substance thereby obtained
  8. 8
    其他was purified by silica gel column chromatography (n-hexane/ethyl acetate=10/1)

实验过程

A mixture comprising 2.1 g of 4-formyl-5-hydroxy-3-methylbenzothiophene, 2.4 g of 4,6-dimethoxy-2-methylsulfonylpyrimidine and 1.8 g of potassium carbonate in 30 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for 3 hours. The mixture was returned to room temperature, then poured into water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. Then, it was concentrated under reduced pressure, and the oily substance thereby obtained was purified by silica gel column chromatography (n-hexane/ethyl acetate=10/1) to obtain 3.1 g (yield: 86%) of the desired compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05616537uspto-grants-1997_04