تفاعل #66689

ord-1df77548902c412289a0d4218c428ab1

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGto stir for 17 hours at room temperature
  2. 2
    تركيزThe reaction mixture was concentrated to 200 mL volume under reduced pressure
  3. 3
    workup.ADDITIONpoured onto ice
  4. 4
    أخرىSolids were removed by filtration
  5. 5
    غسيلwashed with brine
  6. 6
    تجفيفdried (MgSO4)
  7. 7
    ترشيحfiltered
  8. 8
    أخرىevaporated 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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524725B2uspto-grants-2013_09