HRID1068168

反应详情

EQUATION

反应方程式

HRID 1068168 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (1-Benzyl-piperidin-4-yl)-(3-nitro-pyridin-2-yl)-amine (from Step A) in 10 mL of THF was added 2.4 g of SnCl2 and 1 mL of concentrated HCl at room temperature, stirred at room temperature for 2 hours. The reaction was diluted with 40 mL of EtOAc and washed with 30 mL of saturated NaHCO3 aqueous solution. After separating layers, the aqueous phase was extracted with 2×15 mL EtOAc. The combined organic phases were washed with 15 mL of brine, dried over MgSO4 and concentrated under reduced pressure to give 603 mg of yellow soid.

WORKUP

后处理

  1. washwashed with 30 mL of saturated NaHCO3 aqueous solution
  2. customAfter separating layers
  3. extractionthe aqueous phase was extracted with 2×15 mL EtOAc
  4. washThe combined organic phases were washed with 15 mL of brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customto give 603 mg of yellow soid