반응 #89751

ord-8a028f4803844a06b97490d17c5d9695

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After quenched with water
  2. 2
    추출the mixture was extracted with ethyl acetate
  3. 3
    세척The combine organic lyers were washed with brine
  4. 4
    기타dried
  5. 5
    농축concentrated
  6. 6
    기타to dry
  7. 7
    기타The residue was used directly in next step without further purification

실험 절차

To a mixture of (2S,3S,5S)-5-methoxy-3-(methoxycarbonyl)piperidine-2-carboxylic acid (14.0 mg, 0.0000644 mol), 1-phenyl-piperazine (0.01231 mL, 8.056E-5 mol) and benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (35.63 mg, 8.056E-5 mol) in N,N-dimethylformamide (0.20 mL, 0.0026 mol) was added N,N-diisopropylethylamine (0.01403 mL, 8.056E-5 mol). The mixture was stirred at rt for 2 h. After quenched with water, the mixture was extracted with ethyl acetate. The combine organic lyers were washed with brine, dried and concentrated to dry. The residue was used directly in next step without further purification. MS (ESI): (M+H)+=362.1.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440958B2uspto-grants-2016_09