反応 #2254183

反応方程式

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

収率 111.4%

溶媒

THF

反応条件

後処理

1. 1
   workup.ADDITIONthe reaction mixture is poured onto water (500 ml) at 0° C
2. 2
   抽出The organic phase is extracted with water
3. 3
   乾燥a saturated aqueous solution of NaCl, dried over Na2SO4
4. 4
   濃縮concentrated in vacuo

実験手順

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.

出典