2-AMINO-N-CYCLOHEXYL-N-METHYLBENZENE METHAMINE HCL synthesis

Yield: 85%

Reaction Conditions:

in ethanol at 20; for 1.5 h;Reflux;Time;Solvent;

Steps:

1.2; 2.2; 3.2; 4.2; 5.2 Step 2: Synthesis of impurity C
Under the temperature control of 30, add 11g compound 1 to 33ml of N-methylcyclohexylamine in 30min in batches. After the addition, stir at room temperature for 1h, add 27ml of absolute ethanol, heat to reflux, and decolorize the activated carbon for 20min. After pressure-evaporating the solvent, the oil pump evaporates the remaining N-methylcyclohexylamine to obtain 14.42 g of bromhexine hydrochloride impurity C with a yield of 85.0percent and a purity of 98.85percent

References:

Hebei Yuchen Pharmaceutical Technology Co., Ltd.;He Qingguo;Sun Shuling;Guo Yanli;Meng Zhou;Liu Ruixin;Yang Yawei;Jia Cong;Song Xiangzhi CN111533661, 2020, A Location in patent:Paragraph 0039-0040; 0044-0045; 0049-0050; 0054-0055