تفاعل #94530

ord-eb10d7c1a1e14f47b5cccd80dd7a2c25

معادلة التفاعل

CCC1(C)CCC(C)C(C)(CC)N1
2,6-diethyl-2,3,6-trimethylpiperidine
C=CC(=O)Cl
acrylic chloride
CCN(CC)CC
triethylamine
C=CC(=O)N1C(C)(CC)CCC(C)C1(C)CC
1-acryloyl-2,6-diethyl-2,3,6-trimethylpiperidine

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITis continued for another 24 hours
  2. 2
    درجة الحرارةAfter cooling the reaction mixture
  3. 3
    غسيلis washed twice with 100 ml water each
  4. 4
    تجفيفThe toluene solution is dried over sodium sulfate
  5. 5
    أخرىevaporated
  6. 6
    workup.DISTILLATIONThe residue is distilled in vacuo

الإجراء التجريبي

36.7 g of 2,6-diethyl-2,3,6-trimethylpiperidine (Compound No. 1) are dissolved in 200 ml toluene. A solution of 19 g acrylic chloride in 50 ml toluene is added slowly within an hour and the mixture is stirred at 70°-75° C. for 18 hours. After addition of 21.2 g of triethylamine the stirring is continued for another 24 hours. After cooling the reaction mixture is washed twice with 100 ml water each. The toluene solution is dried over sodium sulfate and evaporated. The residue is distilled in vacuo and there is obtained the 1-acryloyl-2,6-diethyl-2,3,6-trimethylpiperidine (Compound No. 12) as distillate at 133°-135° C./0.6 mm Hg.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04131599uspto-grants-1978_12