反応 #64141

反応方程式

1-(4-bromobenzoyl)-4-(2-hydroxyphenyl)-4-hydroxypiperidine

potassium carbonate

ethylα-bromoisobutyrate

water

→

ethyl 3-{1-(4-bromobenzoyl)-4-hydroxypiperidin-4-yl}α,α-dimethylphenoxyacetate

収率 86.4%

反応条件

後処理

1. 1
   その他After completion of the reaction
2. 2
   温度The reaction mixture was cooled
3. 3
   抽出followed by extraction with chloroform
4. 4
   乾燥Subsequently, the extract was dried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONChloroform and the remained ethyl α-bromoisobutyrate was distilled off under reduced pressure

実験手順

801 mg of {1-(4-bromobenzoyl)-4-(2-hydroxyphenyl)-4-hydroxypiperidine was stirred for 9 hours at the ambient temperature of 100° C. in the presence of 1.20 g (8.68 mmol) of potassium carbonate in 4.00 g (20.5 ml) of ethylα-bromoisobutyrate. After completion of the reaction, The reaction mixture was cooled, and water was added thereto, followed by extraction with chloroform. Subsequently, the extract was dried over anhydrous sodium sulfate. Chloroform and the remained ethyl α-bromoisobutyrate was distilled off under reduced pressure to obtain 902 mg (86.4%) of ethyl 3-{1-(4-bromobenzoyl)-4-hydroxypiperidin-4-yl}α,α-dimethylphenoxyacetate.

出典