HRID1961003
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To a solution of 5-chloro-2-thiophenecarboxylic acid (2.0 g, 12.3 mmol) in dry MeOH (75 mL) was added H2SO4 (1 mL). The reaction mixture was heated to 50° C. for 20 h and was then concentrated under vacuum. The residue was dissolved in DCM and washed several times with saturated NaHCO3 solution. The organic fraction was dried (Na2SO4), concentrated under vacuum and used directly without further purification 21.3 g, quant.): LC-MS (ES) m/z=177 (M+H)+.
WORKUP
后处理
- concentrationwas then concentrated under vacuum
- dissolutionThe residue was dissolved in DCM
- washwashed several times with saturated NaHCO3 solution
- dry with materialThe organic fraction was dried (Na2SO4)
- concentrationconcentrated under vacuum
- customused directly without further purification 21.3 g