تفاعل #94556

ord-957e0430f0bb4036ad303bbdd4622c04

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture is refluxed for 2 hours
  2. 2
    درجة الحرارةcooled
  3. 3
    أخرىquenched slowly with 10N sodium hydroxide
  4. 4
    workup.ADDITIONWater is added
  5. 5
    أخرىthe organic layer is separated
  6. 6
    غسيلwashed 3 times with water
  7. 7
    تجفيفdried over sodium magnesium sulfate
  8. 8
    أخرىRemoval of the solvent
  9. 9
    أخرىyields an off-white solid, mp 88°-92° C.

الإجراء التجريبي

A 16.60 g portion of 3-(p-chlorobenzoyl)-1-(p-chlorophenyl)-3-azabicyclo[3.1.0]hexane (prepared above) is dissolved in 160 ml of benzene and 55.5 g of sodium bis(2-methoxyethoxy)aluminum hydride (70% benzene solution) is added dropwise. The mixture is refluxed for 2 hours, cooled and quenched slowly with 10N sodium hydroxide. Water is added, the organic layer is separated and washed 3 times with water and then dried over sodium magnesium sulfate. Removal of the solvent yields an off-white solid, mp 88°-92° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04131611uspto-grants-1978_12