تفاعل #2458887

ord-d01da9a8e6f2437aa05f1a407db169ca

معادلة التفاعل

CN1CCC(=C2c3ccccc3C=Cc3ccccc32)CC1
4-(5H-dibenzo[a,d]cyclohepten-5-ylidene)-1-methylpiperidine
CCOC(=O)Cl
ethyl chlorocarbonate
CCOC(=O)N1CCC(=C2c3ccccc3C=Cc3ccccc32)CC1
pale yellow crystals
المردود 94.3%
CCOC(=O)N1CCC(=C2c3ccccc3C=Cc3ccccc32)CC1
Ethyl 4-(5H-dibenzo[a,d]cyclohepten-5-ylidene)-1-piperidinecarboxylate
المردود 94.3%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 3.5 hrs
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    غسيلthe reaction mixture was washed with hydrochloric acid and water
  4. 4
    أخرىdried
  5. 5
    تركيزconcentrated

الإجراء التجريبي

A mixture of 33.0 g of 4-(5H-dibenzo[a,d]cyclohepten-5-ylidene)-1-methylpiperidine, 74.9 g of ethyl chlorocarbonate and 170 ml of toluene was refluxed for 3.5 hrs. After cooling, the reaction mixture was washed with hydrochloric acid and water, and then dried and concentrated. The residue was solidified by treatment with n-hexane to give 37.4 g of pale yellow crystals, which were recrystallized from ethanol to give slightly yellow needles, mp 123°-124° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05095022uspto-grants-1992_03