تفاعل #356684
ord-69dd17d9e2724ff79096b64984e8a2a4
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.ADDITIONAfter the addition
- 2أخرىthe cooling bath was removed
- 3درجة الحرارةThe reaction was cooled with ice-bath
- 4workup.ADDITIONmethanol (100 ml) was added to the reaction mixture
- 5درجة الحرارةwhile maintaining the temperature below 30° C
- 6أخرىThe reaction mixture was evaporated
- 7ترشيحThe solid was collected by vacuum filtration
- 8غسيلwashed with water and hexane
الإجراء التجريبي
2,3-Difluorophenylacetyl chloride(58.1 mmol) in CH2Cl2 (150 ml)was added to a suspension of 5-bromo-1H-pyrrolo[2,3-b]pyridine (8.0 g, 40.6 mmol) and AlCl3 (46 g, 345 mmol) in CH2Cl2 (100 ml) at 0° C. After the addition, the cooling bath was removed and the reaction mixture was stirred at room temperature for 1.5 hrs. The reaction was cooled with ice-bath and methanol (100 ml) was added to the reaction mixture while maintaining the temperature below 30° C. The reaction mixture was evaporated and the residue was suspended in water. The solid was collected by vacuum filtration, washed with water and hexane to give the title compound (14.03 g) in 98% yield.