반응 #92538

ord-25fcdf31b3934f5687f8d846796b100b

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축Then the reaction mixture was concentrated to a residue
  2. 2
    기타partitioned between EA (50 mL) and brine (40 mL)
  3. 3
    기타Organic layer was separated from aqueous layer
  4. 4
    세척washed with brine (50 mL×2)
  5. 5
    건조dried over Na2SO4
  6. 6
    농축concentrated

실험 절차

To a solution of 7-(3-aminophenyl)-2-(4-phenoxyphenyl)pyrazolo[1,5-a]pyrimidine-3-carbonitrile (150 mg, 0.372 mmol) in ethanol (10 mL) was added NaBH4 (70 mg, 1.86 mmol). The mixture was stirred at rt for 16 hr and 60° C. for 2 hr. Then the reaction mixture was concentrated to a residue and partitioned between EA (50 mL) and brine (40 mL). Organic layer was separated from aqueous layer, washed with brine (50 mL×2), dried over Na2SO4 and concentrated to afford 135 mg (crude) of 7-(3-aminophenyl)-2-(4-phenoxyphenyl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carbonitrile as a yellow solid. MS (ESI) m/e [M+1]+ 408.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447106B2uspto-grants-2016_09