反应 #554682

ord-a260ab2c502f4bc79697d6d1ecd379c6

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction mixture was partitioned between EtOAc/brine
  2. 2
    其他the layers separated
  3. 3
    萃取The aqueous layer was extracted with EtOAc (×2)
  4. 4
    干燥the combined organic extracts dried (MgSO4)
  5. 5
    过滤filtered
  6. 6
    浓缩concentrated in vacuo
  7. 7
    其他The residue was triturated from MeCN
  8. 8
    其他the precipitate isolated by filtration

实验过程

2M Na2CO3 (136 μL, 0.272 mmol) was added to a stirred solution of 5-[2-(4-isopropylsulfonylphenyl)-5-(p-tolylsulfonyl)pyrrolo[2,3-b]pyrazin-7-yl]-3-phenyl-isoxazole (40.7 mg, 0.06798 mmol) in THF (4.6 mL) and the reaction stirred at ambient temperature for 64 hours. The reaction mixture was partitioned between EtOAc/brine and the layers separated. The aqueous layer was extracted with EtOAc (×2) and the combined organic extracts dried (MgSO4), filtered and concentrated in vacuo. The residue was triturated from MeCN and the precipitate isolated by filtration to give the title compound as a yellow solid (20.3 mg, 67% Yield). 1H NMR (400.0 MHz, DMSO) δ 1.16 (s, 6H), 3.52 (t, 1H), 7.52-7.61 (m, 4H), 8.02-8.05 (m, 4H), 8.63 (d, 2H), 8.69 (s, 1H), 9.18 (s, 1H) and 13.00 (br s, 1H) ppm; MS (ES+) 445.1.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08623869B2uspto-grants-2014_01