反应详情

To 20 ml of a 2 molar solution of methylamine in tetrahydrofuran chilled in an ice bath was added a solution of 5.16 g of 4-(4-chlorophenyloxy)benzene-sulfonyl chloride in 50 ml of tetrahydrofuran and 20 ml of CH2Cl2. The mixture was refluxed for 2 hours and the solvent removed under vacuum and the residue partitioned between CH2Cl2•H2O (1:1). The CH2Cl2 layer was separated and washed with 2 N citric acid, brine and dried (Na2SO4). The solution was filtered through a thin pad of hydrous magnesium silicate and the filter pad washed with CH2Cl2. The filtrate was concentrated to give 4.5 g of N-methyl-4-(4-chlorophenoxy)benzene-sulfonamide as a yellow solid, m.p. 80-83° C.

1. temperatureThe mixture was refluxed for 2 hours
2. customthe solvent removed under vacuum
3. customthe residue partitioned between CH2Cl2•H2O (1:1)
4. customThe CH2Cl2 layer was separated
5. washwashed with 2 N citric acid, brine
6. dry with materialdried (Na2SO4)
7. filtrationThe solution was filtered through a thin pad of hydrous magnesium silicate
8. washthe filter pad washed with CH2Cl2
9. concentrationThe filtrate was concentrated