HRID438030
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 0.15 mole each of diphenyl phenylphosphonite, acetaldehyde, and p-toluenesulfonamide in 100 g of chlorobenzene is stirred and warmed at 103°-115° C. for 1 hr, and the solvent and by-product phenol are removed by concentration of the reaction mixture to 120° at 0.5 mm. Ether is stirred into the residue, causing separation of 49.4g (79% yield) of solid product. Recrystallization twice from chlorobenzene gives a white solid: mp 178°-181°; 31P nmr (DMSO-d6)- 37.7 ppm.
WORKUP
后处理
- temperaturewarmed at 103°-115° C. for 1 hr
- customthe solvent and by-product phenol are removed by concentration of the reaction mixture to 120° at 0.5 mm
- stirringEther is stirred into the residue