تفاعل #89756

ord-d4e3a1a9804049138007034ff1f6ec5a

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter quenched with aq. sodium bicaronate
  2. 2
    استخلاصthe reaction was extracted with ethyl acetate
  3. 3
    غسيلThe combined organic layers were washed with brine
  4. 4
    أخرىdried
  5. 5
    تركيزconcentrated
  6. 6
    أخرىto dry

الإجراء التجريبي

To a mixture of methyl(2S,3S,5S)-5-tert-butoxy-2-[(4-phenylpiperazin-1-yl)carbonyl]piperidine-3-carboxylate (0.03345 g, 8.290E-5 mol) and 4-dimethylaminopyridine (0.0152 g, 0.000124 mol) in methylene chloride (1.50 mL, 0.0234 mol) was added methyl chloroformate (0.00833 mL, 0.000108 mol). The reaction was stirred at rt overnight. After quenched with aq. sodium bicaronate, the reaction was extracted with ethyl acetate. The combined organic layers were washed with brine, dried, concentrated to dry. The resulting residue was used directly in next step. MS (ESI): (M+H)+=462.2.

المصدر

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