반응 #155758

반응 방정식

MTBE

LiH

2,2,2-trifluoro-1-(3,4,5-trichloro-phenyl)-ethanone

5-acetyl-2-methyl-furan-3-carboxylic acid methyl ester

→

2-methyl-5-[4,4,4-trifluoro-3-hydroxy-3-(3,4,5-trichloro-phenyl)-butyryl]-furan-3-carboxylic acid methyl ester

수율 123.5%

용매

THF

반응 조건

후처리

1. 1
   workup.ADDITIONthe reaction mixture is poured onto water (750 ml) at 0° C
2. 2
   세척The organic phase is washed with water
3. 3
   건조a saturated aqueous solution of NaCl dried over MgSO4
4. 4
   농축concentrated in vacuo

실험 절차

LiH (1.76 g) is added to a solution of 2,2,2-trifluoro-1-(3,4,5-trichloro-phenyl)-ethanone (35.33 g) and 5-acetyl-2-methyl-furan-3-carboxylic acid methyl ester (20 g) in THF (300 ml). After 1 hour 30 at 60° C. MTBE is added (450 ml) and the reaction mixture is poured onto water (750 ml) at 0° C. The organic phase is washed with water and a saturated aqueous solution of NaCl dried over MgSO4 and concentrated in vacuo to yield 62.3 g of 2-methyl-5-[4,4,4-trifluoro-3-hydroxy-3-(3,4,5-trichloro-phenyl)-butyryl]-furan-3-carboxylic acid methyl ester. The crude product is used without further purification. MS (HPLC/MS): 459 (MH+).

출처