反应 #417974

反应方程式

potassium carbonate

3-cyanobenzoic acid

hydroxylammonium chloride

→

3-(N-hydroxycarbamimidoyl)benzoic acid

溶剂

methanol

反应条件

后处理

1. 1
   温度The reaction mixture is then heated at the boil for 15 hours
2. 2
   其他The reaction mixture is evaporated in vacuo
3. 3
   workup.DISSOLUTIONthe residue is dissolved in water
4. 4
   其他The precipitate formed
5. 5
   过滤is filtered off with suction
6. 6
   洗涤washed with water
7. 7
   其他dried in vacuo

实验过程

1382 g (10.0 mol) of potassium carbonate are added in portions with stirring to a suspension, kept 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, the residue is dissolved in water and acidified using 37% aqueous hydrochloric acid. The precipitate formed is filtered off with suction, washed with water and dried in vacuo: 3-(N-hydroxycarbamimidoyl)-benzoic acid as colourless crystals; m.p. 208°; ESI 181 (M+H).

来源