تفاعل #76214
ord-3bf23ac72d0e454e87c0e21c7a1e4332
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةwas heated
- 2درجة الحرارةunder reflux
- 3تركيزThe reaction mixture was concentrated
- 4workup.ADDITIONpoured into water (1 L)
- 5ترشيحThe precipitated solid was collected by filtration
- 6غسيلwashed with water
- 7تجفيفwith isopropyl ether, air-dried
- 8أخرىfurther 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.