HRID1510249

反应详情

EQUATION

反应方程式

HRID 1510249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-anilino-N-[4-(4-pyridinyl)phenyl]acetamide (40.0 mg) in dichloromethane (0.80 mL) were added pyridine (0.0533 mL) and methylsulfonyl chloride (0.0204 mL) at 0° C. and the mixture was stirred at ambient temperature for 2 days. Water (4.0 mL) was added to the mixture at ambient temperature and the mixture was extracted with ethyl acetate (6.0 mL). The organic layer was washed successively with saturated sodium bicarbonate aqueous solution and brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by preparative thin-layer chromatography (4% methanol in chloroform) to afford 2-[(methylsulfonyl)(phenyl)amino]-N-[4-(4-pyridinyl)phenyl]acetamide (31.4 mg) as white crystals.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate (6.0 mL)
  2. washThe organic layer was washed successively with saturated sodium bicarbonate aqueous solution and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by preparative thin-layer chromatography (4% methanol in chloroform)