반응 #74648

반응 방정식

HCl

2-iodo-4-(trifluoromethoxy)phenol

potassium carbonate

3-cyano-4-fluoro-N-[1,2,4]thiadiazol-5-yl-benzenesulfonamide

→

title compound

3-cyano-N-(1,2,4-thiadiazol-5-yl)-4-[2-iodo-4-(trifluoromethoxy)phenoxy]benzenesulfonamide

용매

ethyl acetate

Dimethylsulfoxide

반응 조건

후처리

1. 1
   기타The organic layer was collected
2. 2
   세척washed with brine (20 mL)
3. 3
   건조dried over sodium sulphate
4. 4
   농축concentrated in vacuo
5. 5
   기타The residue was triturated in dichloromethane
6. 6
   여과filtered

실험 절차

To a suspension of 2-iodo-4-(trifluoromethoxy)phenol (Preparation 226, 600 mg, 1.97 mmol) and potassium carbonate (1125 mg, 8.14 mmol) in Dimethylsulfoxide (10 mL) was added 3-cyano-4-fluoro-N-[1,2,4]thiadiazol-5-yl-benzenesulfonamide (Preparation 65). The reaction was heated to 80° C. under N2 for 7 hours before the addition of ethyl acetate (20 mL) and 3M aqueous HCl solution (30 mL). The organic layer was collected, washed with brine (20 mL), dried over sodium sulphate and concentrated in vacuo. The residue was triturated in dichloromethane and filtered to afford 965 mg of the title compound.

출처