반응 #10880

반응 방정식

diethylphosphite

triethylamine

2,2-Dibromo-1-[4-(1-piperidinyl)phenyl]ethanone

2,2-dibromo-1-[4-(1-piperidinyl)phenyl]ethanone

→

2-bromo-1-[4-(1-piperidinyl)phenyl]ethanone

수율 100.0%

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   온도The mixture was slowly warmed to room temperature
2. 2
   workup.STIRRINGstirred for 6 h
3. 3
   농축The reaction mixture was concentrated in vacuo
4. 4
   workup.ADDITIONpoured into ice/water
5. 5
   여과The precipitate was collected by filtration
6. 6
   세척washed with water
7. 7
   기타dried in vacuo

실험 절차

2,2-Dibromo-1-[4-(1-piperidinyl)phenyl]ethanone (3 g, 8.3 mmol) (from Step A above) was dissolved in tetrahydrofuran (15 mL), and cooled to 0° C. To the resulting solution were added dropwise diethylphosphite (1.13 mL, 8.7 mmol) and triethylamine (1.21 mL, 8.7 mmol) in tetrahydrofuran (7 mL) at 0° C. with stirring. The mixture was slowly warmed to room temperature and stirred for 6 h. The reaction mixture was concentrated in vacuo and poured into ice/water. The precipitate was collected by filtration, washed with water and dried in vacuo to provide 2-bromo-1-[4-(1-piperidinyl)phenyl]ethanone (2.3 g, 100% yield).

출처