These common heterocyclic compound, 106658-14-4, name is 4-Methoxybenzene-1,2-diamine 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. Formula: C7H11ClN2O
Preparation 21 5-Methoxy-2-mercaptobenzimidazole Refer to Chart H (conversion of H-1 to H-2). To a magnetically stirred solution of 4-methoxy-o-phenylenediamine hydrochloride (20.0 g, 0.115 mol) in 400 ml of ethanol-water (4:1) is added 2 molar equivalent of 85% potassium hydroxide solution and 20 ml of carbon disulfide. The contents are warmed in a 75-80 C. oil bath for 2.5 hours and the solvent is removed in vacuo. To the residual thick slurry is added 200 ml of water, the contents heated to boiling, and 95% ethanol is added until a transparent solution is obtained. The solution is filtered, the filtrate is allowed to stand at 25 C. and the resulting cyrstalline solid is collected, and washed with water-ethanol. Drying in vacuo affords 11.0 g of the titled crystals mp 253-254.2 C. Concentration of the mother liquor and silica chromatography (280 g, acetone-methylene chloride, 1:6) gives an additional 3.9 g of product (total 14.9 g, 72% yield).
The synthetic route of 4-Methoxybenzene-1,2-diamine hydrochloride has been constantly updated, and we look forward to future research findings.
Reference:
Patent; The Upjohn Company; US5077407; (1991); A;,
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