HRID1507464

反应详情

EQUATION

反应方程式

HRID 1507464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Propane-1-sulfonic acid{3-[5-(4-chloro-phenyl)-1-(2,6-dichloro-benzoyl)-1H-pyrrolo[2,3-b]pyridine-3-carbonyl]-2,4-difluoro-phenyl}-amide (0.5 g, 0.8 mmol) were dissolved in 1 ml dimethylformamide 0.1 g sodium carbonate was added under stirring at room temperature. Methyl iodide (70 μl, 0.16 g, 1.1 mmol) was added dropwise under vigorous stirring at room temperature by a syringe. The reaction mixture was stirred at room temperature overnight. Water was added to the stirred suspension, and the mixture was stirred for 1 hour. The reaction mixture was extracted with ethyl acetate twice (2×20 ml). The organic layer was dried over sodium sulfate. After drying of the organic layer, the solvent was evaporated under reduced pressure at 46° C. The brownish remaining crude product was used for the further synthesis without purification.

WORKUP

后处理

  1. additionwas added
  2. stirringunder vigorous stirring at room temperature by a syringe
  3. stirringThe reaction mixture was stirred at room temperature overnight
  4. stirringthe mixture was stirred for 1 hour
  5. extractionThe reaction mixture was extracted with ethyl acetate twice (2×20 ml)
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. customAfter drying of the organic layer
  8. customthe solvent was evaporated under reduced pressure at 46° C
  9. customwas used for the further synthesis without purification