HRID2266410
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 200 °C
PROCEDURE
实验过程
1-(3-Bromo-phenyl)-1H-imidazole-4-carboxylic acid 5 (150 mg, 0.56 mmol) was added to PPA (preheated to 140° C.) and the mixture was stirred until a thick homogeneous solution was obtained. 1,2-Phenyldiamine (67 mg, 0.62 mmol) was added and the mixture was heated for 6 h at 200° C. After cooling to room temperature it was carefully diluted with 6% NH4OH aqueous solution until the pH=8. The precipitate formed was isolated by filtration, dissolved in little ethyl acetate and filtrated again. Concentration of the organic layer afforded 72 mg (38%) of the title compound as a purple solid. HRMS (ESI+): m/z=339.1949 [M+H]
WORKUP
后处理
- customwas obtained
- temperatureAfter cooling to room temperature it
- customThe precipitate formed
- customwas isolated by filtration
- filtrationfiltrated again