반응 #80288

ord-1f7760b0521044bf9540a7fb877206e6

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    기타was returned to room temperature
  3. 3
    추출extracted with ethyl acetate
  4. 4
    세척The organic layer was washed with water
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    기타The residue obtained by concentration under reduced pressure
  7. 7
    기타was crystallized from isopropyl ether

실험 절차

A mixture comprising 2.2 g of benzyl 5-hydroxy-2-methylindol-4-carboxylate, 1.7 g of 4,6-dimethoxy-2-methylsulfonylpyrimidine and 1.3 g of potassium carbonate in 20 ml of N,N-dimethylformamide, was heated and stirred at a temperature of from 70° to 80° C. for two hours. The mixture was returned to room temperature, then poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. The residue obtained by concentration under reduced pressure, was crystallized from isopropyl ether to obtain 2.8 g (yield: 85%) of the desired product. mp: 135°-139° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05616537uspto-grants-1997_04