تفاعل #66689
ord-1df77548902c412289a0d4218c428ab1
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.STIRRINGto stir for 17 hours at room temperature
- 2تركيزThe reaction mixture was concentrated to 200 mL volume under reduced pressure
- 3workup.ADDITIONpoured onto ice
- 4أخرىSolids were removed by filtration
- 5غسيلwashed with brine
- 6تجفيفdried (MgSO4)
- 7ترشيحfiltered
- 8أخرىevaporated under reduced pressure
الإجراء التجريبي
2-Chloro-N-(2,4-dimethoxy-phenyl)-acetamide (45.8 g, 0.2 mol) was dissolved in 1000 mL methylene chloride, and the reaction mixture was stirred at 0° C. under nitrogen. Aluminum trichloride (78.9 g, 0.6 mol) was added in portions over 30 minutes, and the reaction mixture was allowed to stir for 17 hours at room temperature. The reaction mixture was concentrated to 200 mL volume under reduced pressure, and then poured onto ice. Solids were removed by filtration, and the liquid was taken up in EtOAc, washed with brine, dried (MgSO4), filtered, and evaporated under reduced pressure to yield 39.67 g of 2-Chloro-N-(2-hydroxy-4-methoxy-phenyl)-acetamide. MS (M+H)=216.