반응 #90299

반응 방정식

(Z)—N′-hydroxy-2-(trifluoromethyl)nicotinimidamide

3,4-bis(benzyloxy)-5-nitrobenzoic acid

→

(Z)—N′-(3,4-bis(benzyloxy)-5-nitrobenzoyloxy)-2-(trifluoromethyl)nicotinimidamide

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added in one portion
2. 2
   workup.ADDITIONpoured onto water (100 mL)
3. 3
   여과The resulting precipitate was filtered off
4. 4
   세척washed with water
5. 5
   기타dried
6. 6
   기타After recrystallisation from dichloromethane/isopropanol

실험 절차

To a stirred solution of 3,4-bis(benzyloxy)-5-nitrobenzoic acid (0.759 g, 2 mmol) in dimethylformamide (10 mL) at room temperature was added 1,1-carbonyldiimidazole (0.34 g, 2.10 mmol) in one portion. The resulting yellow mixture was allowed to stir for ninety minutes whereupon (Z)—N′-hydroxy-2-(trifluoromethyl)nicotinimidamide (0.41 g, 2 mmol) was added in one portion. The resulting mixture was stifled at room temperature for two hours and then poured onto water (100 mL). The resulting precipitate was filtered off, washed with water and dried. After recrystallisation from dichloromethane/isopropanol, (Z)—N′-(3,4-bis(benzyloxy)-5-nitrobenzoyloxy)-2-(trifluoromethyl)nicotinimidamide was obtained as a light yellow solid, 0.88 g (78%).

출처