تفاعل #61510

ord-32c7f25479d74862932318781f05d062

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas removed under reduced pressure
  2. 2
    أخرىthe residue was partitioned between 30 ml of water and 30 ml of ethyl acetate
  3. 3
    غسيلThe organic layer was washed with saturated Na2CO3 solution, water
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    ترشيحfiltration
  6. 6
    أخرىthe solvent was removed under reduced pressure
  7. 7
    أخرىto yields a white solid

الإجراء التجريبي

To a solution of 5.0 g Piperidin-4-yl-carbamic acid tert-butyl ester in 15 ml methanol 7.34 ml acetone, 3.14 g Na(CN)BH3 and 0.3 ml acetic acid were added. After stirring for 16 h at RT the solvent was removed under reduced pressure and the residue was partitioned between 30 ml of water and 30 ml of ethyl acetate. The organic layer was washed with saturated Na2CO3 solution, water and then dried over Na2SO4. Following filtration, the solvent was removed under reduced pressure to yields a white solid. Yield: 4.8 g MS (ES+): m/e=243.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07429581B2uspto-grants-2008_09