HRID30464

反应详情

EQUATION

反应方程式

HRID 30464 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 6-chloronicotinic acid (0.985 g, 6.25 mmol) and 1-isopropyl-piperazine (1.50 g, 7.50 mmol) in DCM (100 mL) was added HOBt (1.20 g, 9.40 mmol), EDC (1.80 g, 9.40 mmol), and N-methyl morpholine (3.4 mL, 31.3 mmol). After 18 h the reaction was diluted with 1 N NaOH (50 mL) and extracted with DCM (3×50 mL). The organic extracts were combined, dried (Na2SO4), and concentrated. Chromatography of the residue (SiO2: 2-4% 2 M NH3 in MeOH/DCM) gave the title compound as a solid (0.934 g, 56%).

WORKUP

后处理

  1. extractionextracted with DCM (3×50 mL)
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated