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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A mixture of the compound 2,4-dichloro-1,3,5-triazine (267 mg, 1.78 mmol) and solid K2CO3 (1.23 g, 8.42 mmol) was suspended in AcCN (20 mL) under nitrogen at 0° C. followed by addition of a solution of 1-pyridin-2-ylmethyl-1H-indazol-5-ylamine (Step 3) (400 mg, 1.78 mmol) in AcCN (3 mL) over 5 min. The mixture was stirred at 0° C. for 1 h. The reaction was quenched by pouring onto water. The organics were extracted into EtOAc (200 mL), washed with brine, dried over anh. Na2SO4, concentrated under reduced pressure then purified by column chromatography (elution with EtOAc followed by 9:1 CH2Cl2/MeOH) to give (4-chloro-[1,3,5]triazin-2-yl)-(1-pyridin-2-ylmethyl-1H-indazol-5-yl)-amine.
WORKUP
后处理
- customThe reaction was quenched
- additionby pouring onto water
- extractionThe organics were extracted into EtOAc (200 mL)
- washwashed with brine
- dry with materialdried over anh. Na2SO4
- concentrationconcentrated under reduced pressure
- customthen purified by column chromatography (elution with EtOAc followed by 9:1 CH2Cl2/MeOH)