تفاعل #76214

ord-3bf23ac72d0e454e87c0e21c7a1e4332

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةunder reflux
  3. 3
    تركيزThe reaction mixture was concentrated
  4. 4
    workup.ADDITIONpoured into water (1 L)
  5. 5
    ترشيحThe precipitated solid was collected by filtration
  6. 6
    غسيلwashed with water
  7. 7
    تجفيفwith isopropyl ether, air-dried
  8. 8
    أخرىfurther dried under reduced pressure at 40° C.

الإجراء التجريبي

A mixture of 2-bromo-3′,4′-dichloroacetophenone (78.0 g), sodium formate (68.0 g) and methanol (300 mL) was heated under reflux and stirred for 16 h. The reaction mixture was concentrated and poured into water (1 L). The precipitated solid was collected by filtration, washed with water and then with isopropyl ether, air-dried, and further dried under reduced pressure at 40° C. to give the title compound as crystals (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale-yellow prism crystals. melting point: 115-118° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06699995B1uspto-grants-2004_03