تفاعل #49081

ord-e0566abf77a540a89a8c485236349865

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITat room temperature for 66 hours
  2. 2
    أخرىtimes 0.78 and 1.06 min.

الإجراء التجريبي

The title compound (13.4 g, 94%) was prepared from 2-methyl-2-(1-pyrrolidinyl)butanenitrile D21 (9.6 g, 0.063 mol) and phenyllithium in dibutylether (63 ml of a 2M solution; 0.126 mol) in THF (200 ml), followed by reaction with sodium borohydride (3.5 g, 0.092 mol) in methanol (200 ml) in a similar manner to that described in D5, except that after addition of the sodium borohydride stirring was continued with ice cooling for 0.5 hours then at room temperature for 66 hours. Mass spectrum (Electrospray LC/MS), ES+: Found 233 (MH+). C15H24N2 requires 232. Ret. times 0.78 and 1.06 min.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745642B2uspto-grants-2010_06