Réaction #2254183
ord-ab928e0f26884264b9272187ac83b3b2
Équation de réaction
MTBE
LiH
3′,5′-dichloro-2,2,2-trifluoroacetophenone
1-(5-bromo-4-methyl-thiophen-2-yl)-ethanone
→
1-(5-bromo-4-methyl-thiophen-2-yl)-3-(3,5-dichloro-phenyl)-4,4,4-trifluoro-3-hydroxy-butan-1-one
Rendement 111.4%
Réactifs
Réactifs
Aucun
Solvants
Conditions de réaction
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1workup.ADDITIONthe reaction mixture is poured onto water (500 ml) at 0° C
- 2ExtractionThe organic phase is extracted with water
- 3Séchagea saturated aqueous solution of NaCl, dried over Na2SO4
- 4Concentrationconcentrated in vacuo
Mode opératoire
LiH (2.06 g) is added to a solution of 3′,5′-dichloro-2,2,2-trifluoroacetophenone (48.0 g) and 1-(5-bromo-4-methyl-thiophen-2-yl)-ethanone (30.3 g) in THF (1000 ml). After 2 hours at 60° C. MTBE is added (300 ml) and the reaction mixture is poured onto water (500 ml) at 0° C. The organic phase is extracted with water and a saturated aqueous solution of NaCl, dried over Na2SO4 and concentrated in vacuo to yield 71.2 g of 1-(5-bromo-4-methyl-thiophen-2-yl)-3-(3,5-dichloro-phenyl)-4,4,4-trifluoro-3-hydroxy-butan-1-one. The crude product is used without further purification.