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
Under an atmosphere of argon gas, a solution of dimethyl methylphosphonate (DMMP; 147 g) in anhydrous toluene (1500 ml) was cooled to −74° C. Thereto, n-butyllithium (714 ml; 1.52 M in hexane) was added for 1 hour. The mixture was stirred for 1 hour. Thereto, a solution of N-methoxy-N-methyl-(3-methoxymethylphenyl)acetic acid amide (200 g; prepared in Reference Example 20) in anhydrous toluene (400 ml) was added for 30 minutes. In addition, the mixture was stirred for 2 hours. Thereto, acetic acid (73.5 ml) was added. The mixture was heated to room temperature and poured into water. The organic layer was separated. The organic layer was washed by water and an aqueous saturated solution of sodium chloride successively, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography to obtain the title compound (206.5 g).
WORKUP
后处理
- stirringIn addition, the mixture was stirred for 2 hours
- customThe organic layer was separated
- washThe organic layer was washed by water
- dry with materialan aqueous saturated solution of sodium chloride successively, dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified with silica gel column chromatography