تفاعل #94832

ord-bb7ba48008e44d2aadc07ecb88464455

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthen heated
  2. 2
    درجة الحرارةat reflux for 21/2 hours
  3. 3
    درجة الحرارةAfter cooling the mixture
  4. 4
    أخرىwas quenched with 150 ml of methanol
  5. 5
    workup.ADDITIONAn excess of 10% hydrochloric acid was added
  6. 6
    درجة الحرارةby heating on the steambath for 2 hours
  7. 7
    درجة الحرارةAfter cooling
  8. 8
    workup.ADDITIONether was added
  9. 9
    أخرىevaporated
  10. 10
    استخلاصextracted with ether which
  11. 11
    أخرىwas dried
  12. 12
    أخرىevaporated

الإجراء التجريبي

A mixture of 42 g (0.219 m) of the phenylacetonitrile 100 ml of tetrahydrofuran was mixed with 400 ml of 1 molar diborane in tetrahydrofuran then heated at reflux for 21/2 hours. After cooling the mixture was quenched with 150 ml of methanol. After sitting overnight, the mixture was stripped. An excess of 10% hydrochloric acid was added followed by heating on the steambath for 2 hours. After cooling, ether was added. The mixture was stirred for 1/2 hour and evaporated. The remaining aqueous layer was made basic with 10% sodium hydroxide, extracted with ether which was dried and evaporated to give 2-methyl-3,4-dimethoxyphenethylamine.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04342686uspto-grants-1982_08