HRID625395

反应详情

EQUATION

反应方程式

HRID 625395 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a 50-mL 3-necked round bottom flask, was placed a solution of N-(3,4-dimethylphenyl)-2-(2-nitro-5-(piperidin-1-yl)phenyl)pyridin-4-amine (300 mg, 0.75 mmol, 1.00 equiv) in tetrahydrofuran/EtOH (10/1 mL), Zn (485 mg, 7.46 mmol, 10.00 equiv), and acetic acid (1 mL). The resulting solution was stirred for 30 min at room temperature. The solids were filtered out. The solution was adjusted to pH 7-8 with sodium bicarbonate (aq). The resulting solution was extracted with 3×25 mL of dichloromethane and the organic layers combined. The resulting mixture was washed with 1×25 mL of brine, dried over sodium sulfate, and concentrated under vacuum. The product was obtained as 270 mg (97%) of a yellow solid.

WORKUP

后处理

  1. customInto a 50-mL 3-necked round bottom flask, was placed
  2. filtrationThe solids were filtered out
  3. extractionThe resulting solution was extracted with 3×25 mL of dichloromethane
  4. washThe resulting mixture was washed with 1×25 mL of brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under vacuum