반응 #1096252

반응 방정식

(2R,3S)-2-(2,4-Difluorophenyl)-3-methyl-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane

5,6-dimethyl-1′,2′,5′,6′-tetrahydro-2,3′-bipyridine

lithium perchlorate trihydrate

→

(2R,3R)-2-(2,4-difluorophenyl)-3-(5,6-dimethyl-5′,6′-dihydro-2,3′-bipyridin-1′(2′H)-yl)-1-(1,2,4-triazol-1-yl)butan-2-ol

수율 35.7%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도refluxed for 40 hours
2. 2
   기타The solvent was evaporated under a reduced pressure
3. 3
   workup.DISSOLUTIONthe thus obtained residue was dissolved in ethyl acetate
4. 4
   세척washed with water
5. 5
   기타The solvent was again evaporated under a reduced pressure
6. 6
   기타the residue was purified
7. 7
   기타to obtain 0.35 g of the intended substance (yield 35.7%)

실험 절차

(2R,3S)-2-(2,4-Difluorophenyl)-3-methyl-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane (0.76 g, 3.0 mmol) and 5,6-dimethyl-1′,2′,5′,6′-tetrahydro-2,3′-bipyridine (3.96 g, 21.0 mmol) were dissolved in acetonitrile (50 ml), and lithium perchlorate trihydrate (1.50 g, 9.3 mmol) was added thereto and refluxed for 40 hours. The solvent was evaporated under a reduced pressure, and the thus obtained residue was dissolved in ethyl acetate and washed with water. The solvent was again evaporated under a reduced pressure, and the residue was purified using a silica gel column to obtain 0.35 g of the intended substance (yield 35.7%).

출처