反应 #90722

反应方程式

HATU

Water

1-methyl-4,5,6,7-tetrahydro-1H-indazole-4-carboxylic acid

(3-chloropyrazin-2-yl)methanamine hydrochloride

→

N-((3-chloropyrazin-2-yl)methyl)-1-methyl-4,5,6,7-tetrahydro-1H-indazole-4-carboxamide

收率 15.0%

溶剂

DCM

反应条件

后处理

1. 1
   workup.STIRRINGThe mixture was stirred at room temperature for 2 hours
2. 2
   其他the DCM layers was separated
3. 3
   洗涤washed with brine
4. 4
   干燥dried over Na2SO4
5. 5
   其他The solvent was removed
6. 6
   其他the residue was purified by column chromatography on silica gel (PE/THF=5/1 v/v %)

实验过程

To a solution of 1-methyl-4,5,6,7-tetrahydro-1H-indazole-4-carboxylic acid (6 g, 33 mmol) and (3-chloropyrazin-2-yl)methanamine hydrochloride (6 g, 33 mmol) in 200 mL of DCM was added TEA (9 g, 88 mmol) dropwise. The resulting mixture was stirred at room temperature for 5 mins, and then HATU (12.5 g, 33 mmol) was added to the solution in portions at 0° C. The mixture was stirred at room temperature for 2 hours. Water was added, the DCM layers was separated, and washed with brine, dried over Na2SO4. The solvent was removed and the residue was purified by column chromatography on silica gel (PE/THF=5/1 v/v %) to afford N-((3-chloropyrazin-2-yl)methyl)-1-methyl-4,5,6,7-tetrahydro-1H-indazole-4-carboxamide (1.5 g, 15%).

来源