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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
1-Oxo-2-methoxy-2-(2-diethylphosphonoethyl)-1,2-diphenylethane (100 g, prepared from benzoin methyl ether and diethyl vinyl phosphonate as described in Example 1 of U.S. Pat. No. 4,082,821) is dissolved in methanol (400 ml). Sodium hydroxide (40 g) is added to the solution and the mixture is heated under reflux for 2 hours. The methanol is removed by rotary evaporation, water (300 ml) is added and the mixture is washed with diethyl ether (4×100 ml). The resulting aqueous mixture is cooled to 0° C., and concentrated hydrochloric acid is added until the pH is zero, when a solid is precipitated. This is washed with water and then stirred together with acetone (300 ml), when sodium chloride remains as undissolved solid. The sodium chloride is filtered off and acetone is removed by evaporation to give a solid which is recrystallised from a mixture of acetone and ether to give 90 g of product, a compound of formula XVIII where R1 is methoxy, R3 and Ar1 are each phenyl, R7 is --CH2CH2 -- and R8 is --CH2CH3.
WORKUP
后处理
- temperaturethe mixture is heated
- temperatureunder reflux for 2 hours
- customThe methanol is removed by rotary evaporation, water (300 ml)
- additionis added
- washthe mixture is washed with diethyl ether (4×100 ml)
- additionconcentrated hydrochloric acid is added until the pH is zero, when a solid
- customis precipitated
- washThis is washed with water
- filtrationThe sodium chloride is filtered off
- customacetone is removed by evaporation
- customto give a solid which
- customis recrystallised from a mixture of acetone and ether