HRID532451
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
- 65 °C
PROCEDURE
实验过程
Tin(II) chloride dihydrate (74.8 g) was added in portions to a solution of 5-bromo-3-nitrothiophene-2-carboxylic acid methyl ester (21.0 g) in methanol (1 L), and the mixture was stirred at 65° C. for 30 min. The mixture was concentrated and 500 mL of ethyl acetate and 700 mL of Rochelle's salt solution were added to the residue. The mixture was vigorously stirred for 1 h. The organic phase was dried over magnesium sulfate and concentrated. The product with the molecular weight of 236.09 (C6H6BrNO2S) was obtained in this way; MS (ESI): 236 (M+H+).
WORKUP
后处理
- concentrationThe mixture was concentrated
- addition500 mL of ethyl acetate and 700 mL of Rochelle's salt solution were added to the residue
- stirringThe mixture was vigorously stirred for 1 h
- dry with materialThe organic phase was dried over magnesium sulfate
- concentrationconcentrated
- customThe product with the molecular weight of 236.09 (C6H6BrNO2S) was obtained in this way