HRID453854

反应详情

EQUATION

反应方程式

HRID 453854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 4-chloro-2-methyl-1H-indole-3-carboxylate (13.45 mmol, 1.0 equiv.) was dissolved in DMF (7 ml) and added at 0° C. to a suspension of NaH (26.90 mmol, 2.0 equiv.) in DMF (13 ml). The mixture was then stirred for 30 min. Methyl iodide (20.17 mmol, 1.5 equiv.) was added dropwise at 0° C. and stirring was carried out for 2 h at 25° C. The reaction mixture was diluted with NH4Cl solution (20 ml) and extracted with ethyl acetate (3×50 ml). The combined organic phases were washed with water and sat. NaCl solution (in each case 50 ml), dried over Na2SO4 and concentrated to dryness under reduced pressure. Yield: 72%

WORKUP

后处理

  1. stirringstirring
  2. waitwas carried out for 2 h at 25° C
  3. extractionextracted with ethyl acetate (3×50 ml)
  4. washThe combined organic phases were washed with water and sat. NaCl solution (in each case 50 ml),
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated to dryness under reduced pressure