تفاعل #1374467

ord-a856183e22964c0a92910b478e8196bc

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرى, the ammonia evaporated
  2. 2
    workup.ADDITIONthe residue added to 1 liter of cold water
  3. 3
    أخرىThe layers are separated
  4. 4
    استخلاصthe aqueous layer is extracted with ether (2 × 300 ml)
  5. 5
    غسيلThe combined ether layers are washed
  6. 6
    أخرىdried
  7. 7
    أخرىevaporated in vacuo

الإجراء التجريبي

A solution of 20.1 g (0.084 moles) of 1-(1,2,3,4-tetrahydrofluoren-2-yl)pyrrolidine, prepared as per Example 7, in 400 ml of tetrahydrofuran and 100 ml of ether is added to 2.5 l of liquid ammonia. 12.25 g (1.72 g-atoms) of lithium ribbon is added over 25 min and the mixture stirred for 15 minutes. 160 ml of ethanol is added over 2.5 hr., the ammonia evaporated and the residue added to 1 liter of cold water. The layers are separated and the aqueous layer is extracted with ether (2 × 300 ml). The combined ether layers are washed, dried and evaporated in vacuo to give 20.2 g of oil of the above title.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US03984419uspto-grants-1976_10