Réaction #76214
ord-3bf23ac72d0e454e87c0e21c7a1e4332
Équation de réaction
Réactifs
Aucun
Solvants
Conditions de réaction
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1Températurewas heated
- 2Températureunder reflux
- 3ConcentrationThe reaction mixture was concentrated
- 4workup.ADDITIONpoured into water (1 L)
- 5FiltrationThe precipitated solid was collected by filtration
- 6Lavagewashed with water
- 7Séchagewith isopropyl ether, air-dried
- 8Autrefurther dried under reduced pressure at 40° C.
Mode opératoire
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.