HRID988976

反应详情

EQUATION

反应方程式

HRID 988976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

LiAIH4 (3.5 equivalents) was suspended in THF and brought to reflux. 2-fluoro-4-methoxy-1-(2-nitro-vinyl)-benzene (1 equivalent) was dissolved in THF and added dropwise to the LiAIH4. The reaction was allowed to proceed at reflux overnight. The reaction was then cooled in an ice bath and H2SO4 was added dropwise. The reaction was extracted with ether. The ether fractions were discarded. The aqueous layer was adjusted to pH 12 with 5% NaOH and extracted with ether (3×). Combined ether fractions were washed with brine and dried over Na2SO4. Solvent was removed to yield 2-(2-fluoro-4-methoxy-phenyl)-ethylamine as an oil, which was used without further purification.

WORKUP

后处理

  1. temperatureto reflux
  2. additionadded dropwise to the LiAIH4
  3. temperatureat reflux overnight
  4. temperatureThe reaction was then cooled in an ice bath
  5. extractionThe reaction was extracted with ether
  6. extractionextracted with ether (3×)
  7. washCombined ether fractions were washed with brine
  8. dry with materialdried over Na2SO4
  9. customSolvent was removed