HRID2267285

反应详情

EQUATION

反应方程式

HRID 2267285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-fluoro-2-nitrobenzene (2 g, 14.2 mmol), tert-butyl 2-aminoethylcarbamate (2.7 g, 17.0 mmol) and triethylamine (1.7 g, 2.4 mmol) in tetrahydrofuran was refluxed for 7 h. After cooling to rt 100 mL of water was added and the mixture was extracted with ethyl acetate (3×100 mL). The combined organic layer was washed with brine (150 mL), dried over anhydrous sodium sulfate and filtered. The solvent was removed and the product was used in the next step without further purification.

WORKUP

后处理

  1. temperaturewas refluxed for 7 h
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate (3×100 mL)
  4. washThe combined organic layer was washed with brine (150 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customThe solvent was removed
  8. customthe product was used in the next step without further purification