Reacción #1193146

Ecuación de reacción

hydrochloric acid

paraldehyde

caustic potash

cyclohexanone

→

2,2'-methylenebiscyclohexanone

Rendimiento 64.0%

Disolventes

methanol

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwas added dropwise to a solution
2. 2
   Otroat 60°-70° C.
3. 3
   Otroof 2 hours
4. 4
   Extracciónextracted with ether
5. 5
   Lavadowashed first with 3% aqueous sodium carbonate
6. 6
   Secadowith saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate
7. 7
   OtroAfter recovering the solvent
8. 8
   workup.DISTILLATIONthe dried product was distilled under vacuum
9. 9
   Otroto provide 340 g (yield: 64%) of a fraction boiling at 135°-145° C./3 mm Hg

Procedimiento

A mixture comprising 68 g of paraldehyde, 6 g of caustic potash and 188 g of methanol was added dropwise to a solution comprising 1,000 g of cyclohexanone and 188 g of methanol at 60°-70° C. over a period of 2 hours, and the resulting mixture was stirred for another 3 hours at 60°-70° C. Thereafter, the reaction mixture was decomposed with dilute hydrochloric acid, extracted with ether, washed first with 3% aqueous sodium carbonate, then with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. After recovering the solvent, the dried product was distilled under vacuum to provide 340 g (yield: 64%) of a fraction boiling at 135°-145° C./3 mm Hg.

Fuente