반응 #79774

ord-6f66962956a94b1cb544567f732d7e9e

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe mixture was stirred at 0° C. for 1 hour
  2. 2
    workup.STIRRINGwith stirring at 0° C
  3. 3
    workup.STIRRINGThe mixture was stirred at ambient temperature for 18 hours
  4. 4
    기타quenched with water (100 ml)
  5. 5
    추출The mixture was extracted with ethyl acetate
  6. 6
    기타The combined extracts were dried
  7. 7
    기타evaporated

실험 절차

4-Amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidine (1.0 g) was added to a mixture of sodium hydride (0.158 g of a 60% dispersion in mineral oil) in dimethyl formamide (70 ml) with stirring under nitrogen at 0° C. The mixture was stirred at 0° C. for 1 hour and then α-bromo-γ-butyrolactone (0.60 g) in dimethylformamide (6 ml) was added dropwise with stirring at 0° C. The mixture was stirred at ambient temperature for 18 hours and then quenched with water (100 ml). The mixture was extracted with ethyl acetate. The combined extracts were dried and evaporated to give 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]-butyrolactone as an oil which was used directly in b).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06713474B2uspto-grants-2004_03