A common heterocyclic compound, 6011-14-9, name is 2-Aminoacetonitrile hydrochloride, molecular formula is C2H5ClN2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 6011-14-9.
General procedure: The aminoacetonitrile hydrochloride was added to a solution of xylene in triethylamine,Heated to 40 for 15 min,Preparation of amino acetonitrile solution;4-trifluoromethylnicotinic acid was dissolved in xylene,Added to the above amino acetonitrile solution,Cooling to -10 C, slowly dropping oxalyl chloride in xylene solution,To be added dropwise,Heated to 45 reaction 1h,Then continue to raise the temperature to 100 reaction 2 h;among them,Aminoacetonitrile hydrochloride and triethylamine in a molar ratio of 1: 2.5; 4-trifluoromethylnicotinic acid and aminoacetonitrile hydrochlorideReaction molar ratio of 1: 0.5; 4-trifluoromethyl nicotinic acid and oxalyl chloride reaction molar ratio of 1: 1.05.After the reaction was completed, the temperature was lowered to 85 C and hot filtration was performed to obtain a filtrate 1 and an organic salt. The resulting filtrate1 slowly cooled to room temperature, transferred to a cryogenic tank, -5 crystallization, filtration,The filtrate 2 (in which N-cyanomethylbis (trifluoromethyl) nicotinamide, flonicamid, 4-trifluoromethylnicotinic acid, xylene and triethylamine was included in the filtrate 2)The filter cake is washed with water,And the volume ratio of 82:18 methyl tert-butyl ether and ethyl acetate solution was recrystallized,A white N-cyanomethylbis (trifluoromethyl) nicotinamide solid powder was obtained,The yield was 71.1% and the purity after purification was 99.9%. Examples 2-5 are respectively a preparation method of N-cyanomethylbis (trifluoromethyl) nicotinamide and N-cyanomethylbisMethyl) nicotinamide, which is similar to the preparation method and application described in Example 1, except that the amount of raw materials involved, the technical parameters involved in the preparation method and the application are different, as follows Table shows:
The synthetic route of 2-Aminoacetonitrile hydrochloride has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Hebei University of Science and Technology; Dong Xinrui; Shu Xueye; Wang Yingnan; Guo Qingchun; Zhang Yue; (17 pag.)CN107286086; (2017); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts