反应 #89764

ord-e5634067d4b04c7a9473d3d6ddd651e9

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture refluxed (oil bath at 85 deg)
  2. 2
    其他Upon completion reaction mixture
  3. 3
    浓缩concentrated in vacuum
  4. 4
    其他The residue was purified by combiflash
  5. 5
    其他to give
  6. 6
    其他the product (53.3 mg, 98% in yield)

实验过程

To a stirred solution of methyl(3R,4S)-1-[(Z)-(cyanoimino)(phenoxy)methyl]-4-[4-(4-cyano-2-methylphenyl)piperazin-1-yl]carbonylpiperidine-3-carboxylate (52 mg, 0.00010 mol) in acetonitrile (2.006 mL, 0.03840 mol) was added piperidine (0.200 mL, 0.00202 mol). The reaction mixture refluxed (oil bath at 85 deg). Upon completion reaction mixture concentrated in vacuum. The residue was purified by combiflash using 0-5% methanol/dichloromethane to give the product (53.3 mg, 98% in yield). MS (ESI): (M+H)+=506.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09440958B2uspto-grants-2016_09