HRID924362

反应详情

EQUATION

反应方程式

HRID 924362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 20 mL microwave vial containing 4-chloro-3-nitropyridine (Aldrich, 1.373 g, 8.660 mmol) and benzyl (3S)-piperidin-3-ylcarbamate (MolBridge, 2.077 g, 8.865 mmol), 1-butanol (10.0 mL) was added followed by DIPEA (1.836 g, 14.20 mmol). The mixture was irradiated with microwaves at 130° C. for 1 h. The mixture was then concentrated under reduced pressure, and the resulting residue was purified by flash chromatography on silica gel (0-30% MeOH in DCM) to give the sub-title compound as a yellow solid (2.96 g, 96%). LCMS calc. for C18H21N4O4 (M+H)+: m/z=357.2. found 357.1.

WORKUP

后处理

  1. additionwas added
  2. customThe mixture was irradiated with microwaves at 130° C. for 1 h
  3. concentrationThe mixture was then concentrated under reduced pressure
  4. customthe resulting residue was purified by flash chromatography on silica gel (0-30% MeOH in DCM)