HRID2407817
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
To a stirred solution of the compound prepared in Example 421 (1.88 g) in N,N-dimethylformamide (25 mL) was added N,N-dimethylformamide dimethylacetal (1.61 mL) at room temperature. The resulting purple solution was placed in an oil bath and heating was started to 140° C. The mixture was heated for 30 minutes, cooled to room temperature, the solvent evaporated in vacuo, coevaporated from methanol and dried further under high vacuum for 2 hours. This material was triturated in 1:1 hexane-ether and collected by filtration to afford the title compound as red solids (2.2 g) with the following physical data.
WORKUP
后处理
- customThe resulting purple solution was placed in an oil bath
- temperatureheating
- customwas started to 140° C
- temperatureThe mixture was heated for 30 minutes
- customthe solvent evaporated in vacuo
- customdried further under high vacuum for 2 hours
- customThis material was triturated in 1:1 hexane-ether
- filtrationcollected by filtration