production method | starting from methylamine, obtained by addition, cyclization, hydrolysis and elimination. 1. Addition a 40% methylamine solution was heated to produce methylamine gas. After drying, methyl acrylate was introduced with stirring and reacted at a temperature below 50 °c. After completion, the mixture was stirred at room temperature for another 2 hours, the low boiling substance was removed under reduced pressure, and then distilled under reduced pressure to collect 108-112 ° C. (0.267-0.40kPa) fraction to give N-methyl-N,N-bis (β-methoxycarbonylethyl) amine (adduct). 2. Cyclization the methanol in the sodium methoxide methanol solution is distilled off, and when sodium methoxide crystals are precipitated, toluene is added, and the remaining methanol is fractionated by heating. The mixture was cooled to 70 °c and the adduct was added dropwise with stirring. The reaction temperature was 70-85 °c. After completion of the addition, the methanol was distilled off until the temperature at the top of the fractionation column reached 110 ° C., and the cyclization was performed to form 1-methyl-3-methoxycarbonylpiperidone-[4]. 3. Hydrolysis and elimination the above-mentioned cyclo-compounds were cooled to 5 ℃, vigorously stirred, concentrated hydrochloric acid pre-cooled to 5 ℃ was quickly added, and then allowed to stand and layered, and the toluene layer was extracted with 20% hydrochloric acid solution, the extract was combined with the acid layer and heated to reflux with stirring until no more carbon dioxide occurred. Distillation under reduced pressure to near dryness gave 1-methyl-4-piperidone hydrochloride. |