反应详情

A solution of 0.015 mole of lithium N,N-diisopropylamide (prepared as in example 55) in tetrahydrofuran is chilled to -65° C to -75° C. To the solution is added methyl (4-chloro-3-methylphenoxy)[p-(p-chlorophenoxy)phenyl]acetate in tetrahydrofuran. To the mixture is added 5 ml of hex amethylphosphoramide and while chilling to -65° C to -75° C, 4.26 g of methyl iodide is added. After 1 hr., the mixture is allowed to warm to room temperature and stir overnight. The mixture is poured into water and extracted with ether. The ether extracts are washed with 10% hydrochloric acid, water, saturated NaHCo3, saturaed NaCl solution and dried (MgSO4). Evaporation of the solvent under reduced pressure gives the product as an oil.

1. temperaturewhile chilling to -65° C to -75° C
2. extractionextracted with ether
3. washThe ether extracts are washed with 10% hydrochloric acid, water, saturated NaHCo3, saturaed NaCl solution
4. dry with materialdried (MgSO4)
5. customEvaporation of the solvent under reduced pressure