HRID634708
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
PROCEDURE
实验过程
A mixture of 6-methoxy-7-(2-(4-methylpiperazin-1-yl)ethoxy)-3,4-dihydroquinazolin-4-one (500 mg, 1.57 mmol), thionyl chloride (20 ml) and DMF (3 drops) was heated at reflux for 3 hours and allowed to cool. The excess thionyl chloride was removed by evaporation, and the residue was azeotroped with toluene. The residue was treated with aqueous sodium hydrogen carbonate and the product was extracted with methylene chloride. The combined extracts were washed with brine, passed through phase separating paper and the solvent removed by evaporation to give 4-chloro-6-methoxy-7-(2-(4-methylpiperazin-1-yl)ethoxy)quinazoline (120 mg, 23%).
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for 3 hours
- temperatureto cool
- customThe excess thionyl chloride was removed by evaporation
- customthe residue was azeotroped with toluene
- additionThe residue was treated with aqueous sodium hydrogen carbonate
- extractionthe product was extracted with methylene chloride
- washThe combined extracts were washed with brine
- customseparating paper
- customthe solvent removed by evaporation