反応 #74648

反応方程式

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

溶媒

ethyl acetate

Dimethylsulfoxide

反応条件

後処理

1. 1
   その他The organic layer was collected
2. 2
   洗浄washed with brine (20 mL)
3. 3
   乾燥dried over sodium sulphate
4. 4
   濃縮concentrated in vacuo
5. 5
   その他The residue was triturated in dichloromethane
6. 6
   ろ過filtered

実験手順

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.

出典