HRID2233907
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of methyl 2,4-dichloropyrimidine-6-carboxylate (commercially available) (0.95 g, 4.6 mmol) in DMF (5 ml) was added dropwise to a solution of 3,4-dichloro-5-methyl-N-piperidin-4-yl-1H-pyrrole-2-carboxamide hydrochloride (Intermediate 1, 0.43 g, 4.6 mmol) and TEA (0.92 g, 9.2 mmol) in DMF (10 ml) under nitrogen. The resultant mixture was stirred for 1 h at room temperature. Water (50 ml) was added to the stirred reaction mixture and the material that precipitated was collected and washed with water/acetonitrile (1:1, 15 ml) to give 1.9 g of the title compound. An analytical sample was purified by reversed-phase HPLC (water/acetonitrile gradient, 20-95%).
WORKUP
后处理
- customthe material that precipitated
- customwas collected
- washwashed with water/acetonitrile (1:1, 15 ml)