تفاعل #346130

ord-91f150f7a50b41cf9dc9880206ed3420

الكواشف

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ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITION1 are introduced into a 250 ml three-necked flask
  2. 2
    أخرىequipped with a stirrer
  3. 3
    أخرىis brought to 80° C
  4. 4
    workup.DISSOLUTIONThe initially undissolved catalyst dissolves
  5. 5
    أخرىafter some time triethylamine hydrochloride precipitates
  6. 6
    درجة الحرارةit is first cooled

الإجراء التجريبي

78.1 g (0.5 mol) of caprinaldehyde, 35.1 g (0.5 mol) of methyl vinyl ketone and 13.5 g (0.05 mol) of Cat. 1 are introduced into a 250 ml three-necked flask equipped with a stirrer, reflux condenser (high efficiency, KOH drying tube) and N2 inlet. After adding 40.4 g (0.4 mol) of triethylamine, a N2 atmosphere is set up, the mixture is stirred and the surrounding oil bath is brought to 80° C. The initially undissolved catalyst dissolves and after some time triethylamine hydrochloride precipitates. The mixture is kept at 80° C for 12 hours. For working up, it is first cooled, and then the procedure described in Example 21 is followed. Tetradecane-2,5-dione is obtained. Recrystallization from methanol.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04035395uspto-grants-1977_07