HRID358654

反应详情

EQUATION

反应方程式

HRID 358654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Iodomethane (55.8 ml) was added to a stirred suspension of 2-(2-aminophenyl)-2-oxoethyl benzoate (109 g) and potassium carbonate (1 )8 g) in dry dimethylformamide (400 ml) at ambient temperature. The mixture was stirred at this temperature for 21hours and then at 40° for 5 hours. The solvent was removed under reduced pressure at 60°, water (100 ml) was added and the mixture extracted with dichloromethane (3×200 ml). The combined extracts were dried over sodium sulphate and the solvent was removed by evaporation to leave a dark oil. The oil was purified by flash chromatography on a silica gel column eluted with dichloromethane to give the novel compound 2-[2(methylamino)phenyl]-2-oxoethyl benzoate, m.p. 85°-87°.

WORKUP

后处理

  1. waitat 40° for 5 hours
  2. customThe solvent was removed under reduced pressure at 60°
  3. additionwater (100 ml) was added
  4. extractionthe mixture extracted with dichloromethane (3×200 ml)
  5. dry with materialThe combined extracts were dried over sodium sulphate
  6. customthe solvent was removed by evaporation
  7. customto leave a dark oil
  8. customThe oil was purified by flash chromatography on a silica gel column
  9. washeluted with dichloromethane