HRID79454
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 3-bromo-4-nitro-1H-indazole (Preparation B; 1.00 g, 4.13 mmol) in anhydrous DMF (20 mL) was treated at ambient temperature with potassium carbonate (2.28 g, 16.5 mmol). The reaction mixture was stirred at ambient temperature for 10 minutes and ethyl 2-chloroacetate (0.53 g, 4.34 mmol) was added dropwise. Stirring was continued under nitrogen for 16 hours. The reaction mixture was diluted with excess water and extracted multiple times with DCM and EtOAc. The combined extracts were dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford the product (1.21 g) as a brown solid.
WORKUP
后处理
- stirringStirring
- waitwas continued under nitrogen for 16 hours
- extractionextracted multiple times with DCM and EtOAc
- dry with materialThe combined extracts were dried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure