反应详情

温度

70 °C

Dissolve 1-(3,5-bis-trifluoromethyl-benzyl)-5-chloro-1H-[1,2,3]triazole-4-carboxylic acid ethyl ester in morpholine (20 eq). Stir at 70° C. overnight then increase temp to 80° C. and continue stirring for another 60 hours. Cool to RT, pour into separatory funnel with EtOAc and 1N HCl. Separate layers and wash organic layer with 1N HCl and then with brine. Dry over MgSO4, filter, and concentrate. Purify via silica gel chromatography using a gradient of 1:1 to 1:5 hexanes:EtOAc to give the desired product. MS (IS) 494.2 (M+1). Rf=0.16 (1:1 Hexanes:EtOAc)

1. temperaturethen increase temp to 80° C.
2. stirringcontinue stirring for another 60 hours
3. temperatureCool to RT
4. washSeparate layers and wash organic layer with 1N HCl
5. dry with materialDry over MgSO4
6. filtrationfilter
7. concentrationconcentrate
8. customPurify via silica gel chromatography