反応 #81617

反応方程式

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

溶媒

water

toluene

water

toluene

反応条件

後処理

1. 1
   温度at reflux for 72 hours
2. 2
   ろ過Filter
3. 3
   ろ過through filter aid while at 80° C.
4. 4
   その他separate the organic phase
5. 5
   乾燥Dry (MgSO4)
6. 6
   ろ過filter
7. 7
   その他purify by chromatography (ethyl acetate)

実験手順

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.

出典