HRID74541

反应详情

EQUATION

反应方程式

HRID 74541 的结构方程式

PROCEDURE

实验过程

0.50 g (2.4 mmol) 1-acetyl-4,5-difluoro-1,3-dihydro-indol-2-one were placed in 10 mL DMF under argon. 0.22 g (5.1 mmol) sodium hydride (55%) were added at 0° C. and the reaction mixture was stirred for 1 h. Then 0.32 mL (5.1 mmol) iodomethane were added dropwise. The reaction mixture was stirred overnight at RT, poured onto water and extracted with EtOAc. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was purified by HPLC. The product-containing fractions were combined and concentrated to dryness by rotary evaporation.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred overnight at RT
  2. additionpoured onto water
  3. extractionextracted with EtOAc
  4. customThe organic phase was dried
  5. filtrationfiltered
  6. concentrationconcentrated to dryness by rotary evaporation
  7. customThe residue was purified by HPLC
  8. concentrationconcentrated to dryness by rotary evaporation