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ChemicalBook CAS DataBase List 2-CHLOROETHANIMIDAMIDE HYDROCHLORIDE
20846-52-0

2-CHLOROETHANIMIDAMIDE HYDROCHLORIDE synthesis

3synthesis methods
-

Yield:20846-52-0 988 g

Reaction Conditions:

with sodium methylate;ammonium chloride in methanol at 15 - 20; for 16 h;Inert atmosphere;

Steps:

5 Intermediate 5: 2-Chloro-acetamidine

Sodium (18.3g, 0.795mol) was completely dissolved in 2 L of MeOH at 25 °C and stirred for 1 hour. To the solution was then added chloro-acetonitrile (600 g, 7.95 mol) dropwise in 1 hour under the protection of N2. After being stirred at about 20 °C for an additional hour, NH4Cl (514 g, 8.73 mol) was added in portions over 45 minutes (the solution turned to yellow and then red, and then a black liquid was obtained), the reaction mixture was then allowed to stir at 15-20 °C for 16 hours. After filtration, the filtrate was concentrated to give a residue, which was triturated with MTBE (1 L x 2) to give the title compound as a black solid (988 g, 96%).

References:

WO2013/10092,2013,A1 Location in patent:Page/Page column 28

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