تفاعل #93374

ord-8b99c9550e4f4c0fbace963d499632eb

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling, to the solution
  2. 2
    أخرىThe solvent was removed and to the residue
  3. 3
    workup.ADDITIONwas added water
  4. 4
    استخلاصThe solution was extracted with chloroform
  5. 5
    غسيلthe extract was washed with water
  6. 6
    أخرىdried
  7. 7
    أخرىevaporated
  8. 8
    أخرىThe residue was chromatographed on silica gel using 10% methanol-chloroform as an eluent

الإجراء التجريبي

A solution of 2.80 g of alpha-isopropyl-alpha-[3-[N-[3-(3-hydroxymethylphenoxy)propyl]amino]propyl]-3,4,5-trimethoxyphenyl acetonitrile and 4.84 g of 37% formalin in 70 ml of methanol was refluxed for 1 hour. After cooling, to the solution was added 2.25 g of sodium borohydride and the solution was stirred for 1 hour at room temperature. The solvent was removed and to the residue was added water. The solution was extracted with chloroform and the extract was washed with water, dried, and evaporated. The residue was chromatographed on silica gel using 10% methanol-chloroform as an eluent to give 0.74 g of the desired compound as a yellow oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04612329uspto-grants-1986_09