Yield:15325-51-6 73.3%

Reaction Conditions:

with hydroxylamine hydrochloride;sodium carbonate in ethanol;water at 20; for 14 h;Cooling with ice;Reflux;

Steps:

1.1 Preparation of 1,3-bis-N-hydroxy-benzamidine (A1)

(8.42 g, 80. Ommo 1) was slowly added to water (27 mL) dissolved in hydroxylamine hydrochloride (5.65 g, 81.3 mmol) under ice-cooling, and the mixture was stirred at room temperature Was poured into anhydrous ethanol (30 mL) dissolved in isophthalonitrile (2.56 g, 20. Ommol) and refluxed for 14 h.After cooling to room temperature, place the mixture in a refrigerator (2 to 4 ° C) for 12 h.The resulting solid was washed with water and ethanol and recrystallized from absolute ethanol to give a white solid (2.84 g, 14.6 mmol).The yield was 73.3%

References:

CN103951662,2016,B Location in patent:Paragraph 0067 - 0070