Reaktion #1464288

Reaktionsgleichung

2-methyl-5-(4-chlorobenzylidene)-cyclopentanone

potassium hydroxide

methyl chloride

potassium iodide

→

pale beige solid

Ausbeute 100.1%

2,2-Dimethyl-5-(4-chlorobenzylidene)-cyclopentanone

Ausbeute 100.1%

Lösungsmittel

tert-butanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewere injected at 20° C
2. 2
   workup.DISTILLATION300 ml of tert-butanol were distilled off at 20 mbar up to an overhead temperature of max
3. 3
   Sonstige50° C
4. 4
   workup.ADDITION400 ml of water were added to the residue
5. 5
   workup.STIRRINGthe mixture was stirred thoroughly
6. 6
   FiltrationThe resulting suspension was filtered off over a suction
7. 7
   Filtrationfilter
8. 8
   Waschenthe filter cake was washed twice with 200 ml of water each time
9. 9
   Sonstigedried

Vorschrift

106 g of 2-methyl-5-(4-chlorobenzylidene)-cyclopentanone, 49.5 g of 85% strength aqueous potassium hydroxide solution, 8.3 g of potassium iodide and 400 g of tert-butanol were weighed in succession into a 700 ml stainless steel autoclave, and 50.5 g of methyl chloride were injected at 20° C. The mixture was stirred at room temperature for 23 hours and then 300 ml of tert-butanol were distilled off at 20 mbar up to an overhead temperature of max. 50° C. 400 ml of water were added to the residue, and the mixture was stirred thoroughly. The resulting suspension was filtered off over a suction filter, and the filter cake was washed twice with 200 ml of water each time and dried. 112.8 g of a pale beige solid were thus obtained with a purity of 89.5%. The yield of the crude product was 90.2% of theory.

Quelle