HRID1379300

反应详情

EQUATION

反应方程式

HRID 1379300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturewas cooled in an ice bath
  2. customprepared as in U.S
  3. customThe cooling bath was removed
  4. stirringthe mixture stirred for one hour
  5. customthe layers were separated
  6. washThe organic phase was washed with water (2×100 mL) and brine
  7. dry with materialdried through calcium sulfate