HRID729352

反应详情

EQUATION

反应方程式

HRID 729352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,5-Dinitro-pyridin-4-ylamine 2 (5.00 g, 27 mmol) was suspended in EtOH (80 ml). The flask was evacuated and then purged with a nitrogen atmosphere. To this flask, Pt/C (500 mg of 10%) was added. The flask was re-evacuated, and then placed under a hydrogen atmosphere (40 psi) on a Parr hydrogenator. It was allowed to shake for 18 hours, and was judged complete by TLC. The platinum catalyst was removed by CELITE filtration, and the solvent was removed by evaporation under a reduced atmosphere to yield the title product 3, a brown solid (3.24 g (97%), 27 mmol). 1H NMR (20): δ 7.51 (s, 2H). MS (ESI-POS): [M+H]+=125.

WORKUP

后处理

  1. customThe flask was evacuated
  2. custompurged with a nitrogen atmosphere
  3. additionTo this flask, Pt/C (500 mg of 10%) was added
  4. customThe flask was re-evacuated
  5. customThe platinum catalyst was removed by CELITE filtration
  6. customthe solvent was removed by evaporation under a reduced atmosphere