HRID634697
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 6-methoxy-7-(2-methylthioethoxy)-3,4-dihydroquinazolin-4-one (1.07 g, 4.0 mmol), thionyl chloride (20 ml) and DMF (4 drops) was heated at reflux for 2 hours and then allowed to cool. The excess thionyl chloride was removed by evaporation and the residue was azeotroped with toluene. The solid residue was partitioned between aqueous sodium hydrogen carbonate and methylene chloride, the organic phase was separated and washed with brine. The organic phase was passed through phase separating paper, and the solvent removed by evaporation to give 4-chloro-6-methoxy-7-(2-methylthioethoxy)quinazoline (810 mg, 71%).
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for 2 hours
- temperatureto cool
- customThe excess thionyl chloride was removed by evaporation
- customthe residue was azeotroped with toluene
- customThe solid residue was partitioned between aqueous sodium hydrogen carbonate and methylene chloride
- customthe organic phase was separated
- washwashed with brine
- customseparating paper
- customthe solvent removed by evaporation