반응 #81617

반응 방정식

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

용매

water

toluene

water

toluene

반응 조건

후처리

1. 1
   온도at reflux for 72 hours
2. 2
   여과Filter
3. 3
   여과through filter aid while at 80° C.
4. 4
   기타separate the organic phase
5. 5
   건조Dry (MgSO4)
6. 6
   여과filter
7. 7
   기타purify by chromatography (ethyl acetate)

실험 절차

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.

출처