반응 #80498
ord-fa4a457f5b2f4341835865c0b6b34cb6
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.ADDITIONis added
- 2workup.STIRRINGwhich is stirred at 120° C. for 1 hour
- 3기타On completion of the reaction
- 4온도the reaction solution is cooled to room temperature
- 5추출extracted with toluene
- 6세척The organic layer is washed with water
- 7건조dried over anhydrous magnesium sulfate
- 8농축concentrated under reduced pressure
- 9기타The concentrate is purified by silica gel column chromatography
실험 절차
To 30 ml of N,N-dimethylformamide are added 4-trifluoromethyl phenol (0.77 g) and potassium carbonate (0.72 g) and 5-(4-bromomethyl-3-chlorophenyl)-3(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (1.60 g) is added thereto at room temperature with stirring, which is stirred at 120° C. for 1 hour. On completion of the reaction, the reaction solution is cooled to room temperature, poured into water and extracted with toluene. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography to give 1.50 g of desired compound (refractive index: 1.5961).