Application of 442514-22-9, These common heterocyclic compound, 442514-22-9, name is tert-Butyl (3-(methylamino)propyl)carbamate, 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.
To a solution of tert-butyl (3-(methylamino)propyl)carbamate (8 g, 42.5 mmol) in dichloromethane (DCM) (100 mL) was added TEA (1 1 .85 mL, 85 mmol). The reaction mixture was cooled to 0C and then chloroacetyl chloride (5.1 1 mL, 63.7 mmol) was added dropwise. It was stirred at ambient temperature for 1 h. The reaction was quenched with saturated sodium bicarbonate solution (80 mL) and extracted with DCM (2 x 80 mL). The combined organic layer was washed with brine solution (80 mL), dried over anhydrous Na2S04, filtered and concentrated. The crude residue was purified by flash column chromatography eluting with EtOAc: Hexane (3:7) to give the title compound (7 g, 24.37 mmol, 57.4 % yield) as light yellow liquid. LCMS m/z 265.35 (M+H)+,1 .79 min (ret. time)
The synthetic route of 442514-22-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BOEHM, Jeffrey Charles; DAVIS, Roderick S.; GOODWIN, Nicole Cathleen; KERNS, Jeffrey K.; LI, Tindy; YAN, Hongxing; (113 pag.)WO2018/109648; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics