HRID1164968

反应详情

EQUATION

反应方程式

HRID 1164968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 20.0 9 (0.07 mol) of N-[2-(3,4-dimethoxyphenyl)ethyl]trifluoroacetamide to a suspension of 3.17 g (0.08 mol) of 60% sodium hydride in 50 mL of dry tetrahydrofuran. Stir this suspension for 30 minutes at room temperature. After 30 minutes, add 6.72 mL (0.11 mol) of methyl iodide and stir at room temperature for one h. After one h, filter reaction mixture and make basic (pH=14) with 4N sodium hydroxide. Wash this mixture with 2×100 mL of water. Extract the combined aqueous washes with 2×100 mL of methylene chloride. Wash the combined organic extracts with 6N hydrochloric acid, then with 100 mL of water. Dry the organic layer over anhydrous sodium sulfate. Filter the drying agent and remove the solvent in vacuo to provide the title compound.

WORKUP

后处理

  1. waitAfter 30 minutes
  2. stirringstir at room temperature for one h
  3. filtrationAfter one h, filter
  4. customreaction mixture
  5. washWash this mixture with 2×100 mL of water
  6. extractionExtract the combined aqueous washes with 2×100 mL of methylene chloride
  7. washWash the combined organic extracts with 6N hydrochloric acid
  8. dry with materialDry the organic layer over anhydrous sodium sulfate
  9. filtrationFilter the drying agent
  10. customremove the solvent in vacuo