HRID2423340

反应详情

EQUATION

反应方程式

HRID 2423340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Amino-3-chloro-5-methyl-benzonitrile (499.4 mg, 3.00 mmol) and Borane-THF complex (4 eq, 12.04 mmol, 12.04 ml) were added in THF. The reaction mixture was stirred for 3 hrs in reflux. After confirming the completion of the reaction, MeOH was added slowly added in the mixture. MeOH was removed in vacuo. The residue was extracted with ethyl acetate. A combined organic layer was washed with H2O and brine, dried with Na2SO4, concentrated in vacuo to yield 4-Aminomethyl-2-chloro-6-methyl-phenylamine (19.4 mg), as a yellow syrup.

WORKUP

后处理

  1. temperaturein reflux
  2. additionwas added slowly
  3. additionadded in the mixture
  4. customMeOH was removed in vacuo
  5. extractionThe residue was extracted with ethyl acetate
  6. washA combined organic layer was washed with H2O and brine
  7. dry with materialdried with Na2SO4
  8. concentrationconcentrated in vacuo