تفاعل #10880
ord-ff4256aaf0c04c6c9ceb8c97dc41cecd
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe mixture was slowly warmed to room temperature
- 2workup.STIRRINGstirred for 6 h
- 3تركيزThe reaction mixture was concentrated in vacuo
- 4workup.ADDITIONpoured into ice/water
- 5ترشيحThe precipitate was collected by filtration
- 6غسيلwashed with water
- 7أخرىdried in vacuo
الإجراء التجريبي
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).