Reaktion #643154

Reaktionsgleichung

trimethylphosphonoacetate

DCM

NaH

cyclohexanone

→

title crude product

Methyl 2-cyclohexylideneacetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGstirred at ambient temperature overnight
2. 2
   WaschenThe next day, the reaction mixture was washed with water twice
3. 3
   Trocknensaturated aqueous NaCl solution once, dried over anhydrous MgSO4 for 2 hours
4. 4
   Filtrationfiltrated
5. 5
   Sonstigethe filtrate was dried under vacuum

Vorschrift

2.184 g trimethylphosphonoacetate was dissolved in DCM, stirred on ice-water bath, and 384 mg NaH was added. After 6 hours 980 mg cyclohexanone was added into the reaction flask, and stirred at ambient temperature overnight. The next day, the reaction mixture was washed with water twice, saturated aqueous NaCl solution once, dried over anhydrous MgSO4 for 2 hours, filtrated, and the filtrate was dried under vacuum to give 1.227 g of the title crude product.

Quelle