Electric Literature of 4584-46-7, These common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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 flame-dried two-necked 25 mL round-bottomed flask was charged with cyclic sulfite (1 mmol), Fe3+-clay (100 mg) and dry xylene (5 mL) and stirred under a constant flush of nitrogen. Freshly distilled 2-aminothiophenol (0.9 mmol) was added drop wise, and the reaction mixture was refluxed for 12 h. Crude compound was chromatographed to get cis-(+)-2,3-dihydro-3-hydroxy-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one (50% yield). The hydroxy lactam (0.54 mmol) was dissolved in ethyl acetate (5 mL) and 2-(dimethylamino) ethyl chloride hydrochloride (0.694 mmol) was added followed by addition of finely ground K2CO3 (2.16 mmol) and a drop of water. The heterogeneous mixture was stirred at reflux for 12 h. Solvent was removed and the crude product was chromatographed to obtain N-alkylated product (88%).
The synthetic route of 4584-46-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH; WO2004/58734; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics