Synthetic method for temozolomide intermediate

• Main Authors: DENG ZHIJUN, LIU ZHENDONG, GAN FENGRUI
• Format: Patent
• Language: Chinese; English
• Published: 15.03.2019
• Subjects: CHEMISTRY; HETEROCYCLIC COMPOUNDS; METALLURGY; ORGANIC CHEMISTRY

The invention discloses a synthetic method for a temozolomide intermediate. The temozolomide intermediate is synthesized from 5-aminooimidazole-4-formamide and methylaminoformyl chloride by a one-stepmethod. The synthetic method comprises the following steps: dissolving the 5-aminooimidazole-4-formamide and the methylaminoformyl chloride in an organic solvent, cooling to the temperature of minus5-5 DEG C, dropwise adding triethylamine, heating and keeping stirring for 2-3 h, filtering, washing, and drying for 12 h at the temperature of 50+/- 5 DEG C under vacuum to obtain the temozolomide intermediate. The method is high in safety, use of methyl isocyanate as a highly toxic reagent is avoided, the raw material conversion ratio is high and is 95% or above, the purity of the product is 98.3% or above, the reaction conditions are mild, aftertreatment is simple, and the materials can be fed directly without further purification for next reaction. 本发明公开了种替莫唑胺中间体的合成方法，通过5-氨基咪唑-4-甲酰胺和甲氨基甲酰氯步法合成得到替莫唑胺中间体。将5-氨基咪唑-4-甲酰