HRID555429

反应详情

EQUATION

反应方程式

HRID 555429 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe reaction was flushed with nitrogen
  2. customsealed
  3. temperatureThe reaction was cooled to rt
  4. additiondiluted with EtOAc (˜150 mL)
  5. washwashed twice with saturated aqueous NaCl (2ט150 mL)
  6. extractionThe aqueous washes were then back extracted with EtOAc
  7. dry with materialThe combined organics were dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated