Reference of 15205-11-5, These common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, 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.
Example 91 N-[(2-chloro-4-fluorophenyl)methyl]-5-oxo-1-phenyl-prolinamide (E91) 5-oxo-1-phenyl-proline (0.072 g, 0.35 mmol, prepared as described below) was dissolved in dichloromethane (~2 ml) and dimethylformamide (0.5 ml) and to this was added N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (0.081 g, 0.42 mmol), 1-hydroxybenzotriazole (0.057 g, 0.42 mmol), and N-ethyl morpholine (0.134 ml, 1.05 mmol). The mixture was stirred at room temperature for 30 minutes and then [(2-chloro-4-fluorophenyl)methyl]amine (0.067 g, 0.42 mmol) was added. Stirring was continued overnight at room temperature and then the mixture was diluted with more dichloromethane and saturated aqueous sodium hydrogen carbonate. The aqueous layer was separated and extracted with more dichloromethane (3 aliquots). The combined organic layers were then washed with brine before drying over magnesium sulphate. Evaporation of the solvent then gave a yellow oil which was purified by mass-directed automated HPLC. Finally trituration of the material thus obtained with a 1:1 mixture of dichloromethane and diethyl ether gave, after filtration and drying, pure N-[(2-chloro-4-fluorophenyl)methyl]-5-oxo-1-phenyl-prolinamide (0.031 g) as a white solid. LC/MS [M+H]+=347, retention time=2.46 minutes.
The synthetic route of 15205-11-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXO GROUP LIMITED; US2008/9541; (2008); A1;,
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