Réaction #81617

Équation de réaction

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

Solvants

water

toluene

water

toluene

Conditions de réaction

Traitement

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

Mode opératoire

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.

Source