反应详情

1382 g (10.0 mop of potassium carbonate are added in portions with stirring to a suspension, held at 30° C., of 500 g (3.40 mol) of 3-cyanobenzoic acid in 8 l of methanol. 695 g (10.0 mol) of hydroxylammonium chloride are subsequently added in small portions at an internal temperature of 40-45° C. The reaction mixture is then heated at the boil for 15 hours. The reaction mixture is evaporated in vacuo, and the residue is dissolved in water and acidified using 37% aqueous hydrochloric acid. The resultant precipitate is filtered off with suction, washed with water and dried in vacuo: 3-(N-hydroxycarbamimidoyl)benzoic acid as colourless crystals; m.p. 208° C.; ESI 181 (M+H).

1. temperatureThe reaction mixture is then heated at the boil for 15 hours
2. customThe reaction mixture is evaporated in vacuo
3. dissolutionthe residue is dissolved in water
4. filtrationThe resultant precipitate is filtered off with suction
5. washwashed with water
6. customdried in vacuo