HRID523525

反应详情

EQUATION

反应方程式

HRID 523525 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Zinc powder (223.2 mg, 3.41 mmol) and ammonium chloride solution (365 mg, 6.8 mmol) were added to a stirred solution of 4-cyclopropyl-3-nitropyridine (I-1a: 70 mg, 0.426 mmol) in dry THF (2 mL) at 0° C. and the resulting mixture was stirred at room temperature for 1 hour. The reaction was monitored by TLC (10% methanol in CHCl3). The reaction mixture was filtered over celite bed and washed with THF and filtrate was concentrated. The residue was dissolved in ethyl acetate and washed with water and saturated brine and dried over sodium sulphate and concentrated to afford 450 mg of the product (100% yield).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered over celite bed
  2. washwashed with THF and filtrate
  3. concentrationwas concentrated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with water and saturated brine
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated