反应 #554682
ord-a260ab2c502f4bc79697d6d1ecd379c6
反应方程式
反应物
试剂
溶剂
反应条件
后处理
- 1其他The reaction mixture was partitioned between EtOAc/brine
- 2其他the layers separated
- 3萃取The aqueous layer was extracted with EtOAc (×2)
- 4干燥the combined organic extracts dried (MgSO4)
- 5过滤filtered
- 6浓缩concentrated in vacuo
- 7其他The residue was triturated from MeCN
- 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.