Реакция #417974

Уравнение реакции

potassium carbonate

3-cyanobenzoic acid

hydroxylammonium chloride

→

3-(N-hydroxycarbamimidoyl)benzoic acid

Растворители

methanol

Условия реакции

Обработка

1. 1
   ТемператураThe reaction mixture is then heated at the boil for 15 hours
2. 2
   ДругоеThe reaction mixture is evaporated in vacuo
3. 3
   workup.DISSOLUTIONthe residue is dissolved in water
4. 4
   ДругоеThe precipitate formed
5. 5
   Фильтрацияis filtered off with suction
6. 6
   Промывкаwashed with water
7. 7
   Другоеdried in vacuo

Методика

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).

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