67442-07-3, A common heterocyclic compound, 67442-07-3, name is 2-Chloro-N-methoxy-N-methylacetamide, molecular formula is C4H8ClNO2, 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.
A mixture of 1-benzyl-piperazine (1.0 g, 5.67 mmol), 2-chloro-LambdaA-methylacetamide (671.2 mg, 6.24 mmol, 1.1 eq.), and potassium carbonate (941 mg, 6.81 mmol, 1.2 eq.) in anhydrous THF (23 mL) was stirred at 60 0C under N2 for 18 h. The mixture was cooled to rt and poured into EtOAc. The organic phase was washed with water and brine, dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified by MPLC(Biotage.(R)., gradient elution 1:4:5 v/v MeOH:Acetone:DCM) to give 1.16 g (83percent) of the product as a white solid. 1H-NMR (300 MHz, DMSO-alphafe) .delta 7.62 to 7.56 (broad d, 1H),7.33 to 7.20 (m, 5H), 3.45 (s, 2H), 2.85 (s, 2H), 2.58 (d, 3H), 2.44 to 2.33 (broad s, 8H);ES-MS m/z 248.2 [M+H]+, RT (min) 0.33.
The synthetic route of 67442-07-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BAYER PHARMACEUTICALS CORPORATION; WO2007/56170; (2007); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics