Reaktion #81617

Reaktionsgleichung

4-(4-chloro-1-oxobutyl)-2,2-dimethylphenethyl acetate

α,α-diphenyl-4-piperidinemethanol

potassium hydrogen carbonate

potassium iodide

→

4-[4-[4-(hydroxydiphenylmethyl)-1-piperidinyl]-1-oxobutyl]-2,2-dimethylphenethyl acetate

Lösungsmittel

water

toluene

water

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 72 hours
2. 2
   FiltrationFilter
3. 3
   Filtrationthrough filter aid while at 80° C.
4. 4
   Sonstigeseparate the organic phase
5. 5
   TrocknenDry (MgSO4)
6. 6
   Filtrationfilter
7. 7
   Sonstigepurify by chromatography (ethyl acetate)

Vorschrift

Mix 4-(4-chloro-1-oxobutyl)-2,2-dimethylphenethyl acetate (99.5 g, 0.335 mol), α,α-diphenyl-4-piperidinemethanol (101.8 g, 0.335 mol), potassium hydrogen carbonate (83.8 g, 0.838 mol), potassium iodide (1.00 g, 0.006 mol), toluene (600 mL) and water (220 mL). Stir at reflux for 72 hours, add toluene (200 mL) and deionized water (100 mL). Filter through filter aid while at 80° C. and separate the organic phase. Dry (MgSO4), filter and purify by chromatography (ethyl acetate) to give 4-[4-[4-(hydroxydiphenylmethyl)-1-piperidinyl]-1-oxobutyl]-2,2-dimethylphenethyl acetate as an oily solid.

Quelle