تفاعل #5640

ord-083e912021ea4636b30489d9253b9684

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىTo a 50 mL flask equipped with a condenser
  2. 2
    أخرىdrying tube
  3. 3
    درجة الحرارةThe reaction mixture was heated
  4. 4
    درجة الحرارةto reflux
  5. 5
    أخرىreaction progress
  6. 6
    درجة الحرارةthe mixture was cooled
  7. 7
    غسيلwashed with 50 mL of 5 N NaOH
  8. 8
    استخلاصThe caustic layer was extracted with 3×20 mL of diethyl ether
  9. 9
    تجفيفdried over Na2SO4
  10. 10
    أخرىRemoval of the solvent

الإجراء التجريبي

To a 50 mL flask equipped with a condenser, drying tube and thermometer, was added 1.98 g (0.01 moles) of 4,7-dichloroquinoline, 1.57 g (0.0014 moles) of 4-fluorophenol, 0.22 g (0.0015 moles) of 4-pyrrolidinopyridine and 20 mL of xylene. The reaction mixture was heated to reflux and reaction progress was monitored by TLC. After 18 hr, the mixture was cooled and washed with 50 mL of 5 N NaOH. The caustic layer was extracted with 3×20 mL of diethyl ether. The xylene and the ether layers were combined and dried over Na2SO4. Removal of the solvent provided 2.49 g (91 percent yield) of product, mp=88°-91° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05245036uspto-grants-1993_09