反応 #484787

反応方程式

chlorotriphenylmethane methane

4-piperidone monohydrate hydrochloride

triethylamine

→

1-triphenylmethyl-4-piperidone

収率 103.5%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   workup.STIRRINGthe resulting mixture was stirring further for 5 hours at the same temperature
2. 2
   その他The triethylamine hydrochloride precipitated
3. 3
   温度by cooling
4. 4
   ろ過was filtered out
5. 5
   濃縮the filtrate was concentrated under reduced pressure
6. 6
   workup.ADDITIONTo the residue was added 150 ml of water
7. 7
   抽出followed by extraction with 300 ml of ethyl acetate
8. 8
   洗浄The organic layer was then washed with saturated saline
9. 9
   乾燥dried over anhydrous magnesium sulfate
10. 10
    濃縮The solvent was concentrated under reduced pressure

実験手順

After the portionwise addition of 18.1 g (65.1 mmol) of chlorotriphenylmethane methane to a 150 ml dimethylformamide solution of 10.0 g (65.1 mmol) of 4-piperidone monohydrate hydrochloride and 20.0 g (198 mmol) of triethylamine at 60° C. under stirring, the resulting mixture was stirring further for 5 hours at the same temperature. The triethylamine hydrochloride precipitated by cooling was filtered out and the filtrate was concentrated under reduced pressure. To the residue was added 150 ml of water, followed by extraction with 300 ml of ethyl acetate. The organic layer was then washed with saturated saline and dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure, whereby 23.0 g (yield: 98.3%) of 1-triphenylmethyl-4-piperidone were obtained.

出典