.10 - (beta-morpholine Propionyl) Phenothiazine -2 - Methyl Carbamate Hydrochloride

The synthesis of 10-(β-morpholinylally) phenothiazinel-2-aminoformic acid methylester hydrochloride was investigated and improved in this paper. 3-nitroaniline pasted thereactions of acetylation, condensation, hydrolytic action, reduction, acylation,ring-closure,acylation,arninating,hydrochloride to give 10-(β-morpholinylally)phenothiazinel-2-aminoformic acid methyl ester hydrochloride.Many factors which effect the reaction, such as the reaction time, the reactiontemperature, catalyst as well mole ratios between materials were studied for thecondensation and ring-closure reaction.Under the nitrogen protection, the optimal reaction conditions of the condensationwas that the reaction time was 24 h; the reaction temperature was 163℃; the catalyst waspowder of Cu; the mole ratio of N-(3-nitrophenyl) acetamide to bromobenzene was 1:1.5.The yield of N-acetyl-3-nitrodiphenylamine was 98% under the optimal reactioncondition.For the ring-closure reaction, the optimal reaction conditions was that the dosage ofmethy 3-Nitrodiphenylamine-2-carbamate was 2.00g; the dosage of sulfur was 0.54g; thecatalyst dosage of iodine was.0.08g; the reaction time was 6～7h; the reaction temperaturewas 106℃. The yield of phenothiazinel-2-aminoforrnic acid methyl ester was 78.9%under the optimal reaction condition.