HRID555429
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
- 105 °C
PROCEDURE
实验过程
To a solution of 2-chloro-3-nitrothiophene (1.13 g, 6.93 mmol) in NMP (10 mL) in a pressure vessel was added 2-tert-butylphenol (1.04 g, 6.93 mmol) and K2CO3 (1.0 g, 10.1 mmol). The reaction was flushed with nitrogen, sealed and then heated to 105° C. for 48 h. The reaction was cooled to rt, diluted with EtOAc (˜150 mL) and washed twice with saturated aqueous NaCl (2ט150 mL). The aqueous washes were then back extracted with EtOAc. The combined organics were dried over MgSO4, filtered and concentrated to yield the crude desired product.
WORKUP
后处理
- customThe reaction was flushed with nitrogen
- customsealed
- temperatureThe reaction was cooled to rt
- additiondiluted with EtOAc (˜150 mL)
- washwashed twice with saturated aqueous NaCl (2ט150 mL)
- extractionThe aqueous washes were then back extracted with EtOAc
- dry with materialThe combined organics were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated