تفاعل #985301

ord-dfb84e9f027540deb9d37feb2d5b8c9a

معادلة التفاعل

C1COCCN1
Morpholine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
C#CCBr
propargyl bromide
C#CCN1CCOCC1
colorless oil
المردود 70.0%
C#CCN1CCOCC1
4-Prop-2-ynyl-morpholine
المردود 70.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled in ice under nitrogen
  2. 2
    workup.STIRRINGStirring
  3. 3
    درجة الحرارةwithout cooling
  4. 4
    ترشيحThe white suspension was filtered through paper
  5. 5
    غسيلthe solids were washed with MeOH (100 ml)
  6. 6
    أخرىthe MeOH was carefully evaporated
  7. 7
    ترشيحfiltered through paper
  8. 8
    أخرىcarefully evaporated
  9. 9
    workup.DISTILLATIONFinally the oil was distilled at 60° C./16 mbar

الإجراء التجريبي

Morpholine (100 ml, 1.148 mol) was dissolved in MeOH (1 L) and cooled in ice under nitrogen, then potassium carbonate (120 g, 0.63 mol) and propargyl bromide (124 mL, 1.148 mol) were added while stirring in ice. Stirring without cooling was continued for 4 h. The white suspension was filtered through paper and the solids were washed with MeOH (100 ml) and the MeOH was carefully evaporated. The white precipitate was suspended in DCM (400 ml), filtered through paper, and carefully evaporated. Finally the oil was distilled at 60° C./16 mbar. One obtained 100 g (70%) of a colorless oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07351700B2uspto-grants-2008_04