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 100 mL of toluene, 11.6 g of 50% aqueous sodium hydroxide solution, and 10 mL of water was cooled in an ice bath and treated with 1.3 g of benzyltriethylammonium chloride and 12.0 g of diisopropyl P-(hydroxymethyl)phosphonate (prepared as in U.S. Pat. No. 5,272,128) and stirred vigorously. To this was added a solution of 15 g of the compound of Example 16 (2-trifluoromethyl-6-methylbenzenesulfonyl chloride) in 10 mL of toluene. The cooling bath was removed and the mixture stirred for one hour, then the layers were separated. The organic phase was washed with water (2×100 mL) and brine, then dried through calcium sulfate to yield 23 g of di-O-isopropyl P-[[(2-trifluoromethyl-6-methylphenyl)sulfonyloxy]methyl]phosphonate as a brown oil.
WORKUP
后处理
- temperaturewas cooled in an ice bath
- customprepared as in U.S
- customThe cooling bath was removed
- stirringthe mixture stirred for one hour
- customthe layers were separated
- washThe organic phase was washed with water (2×100 mL) and brine
- dry with materialdried through calcium sulfate