تفاعل #89764

ord-e5634067d4b04c7a9473d3d6ddd651e9

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture refluxed (oil bath at 85 deg)
  2. 2
    أخرىUpon completion reaction mixture
  3. 3
    تركيزconcentrated in vacuum
  4. 4
    أخرىThe residue was purified by combiflash
  5. 5
    أخرىto give
  6. 6
    أخرىthe product (53.3 mg, 98% in yield)

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09440958B2uspto-grants-2016_09