HRID1675723

反应详情

EQUATION

反应方程式

HRID 1675723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

141 mg (0.58 mmol) of 6-bromo-4-chloroquinoline and 150 mg (0.7 mmol) 5-(benzyloxy)-2-methylphenol in 5 ml acetonitrile are mixed with 97 mg (0.7 mmol) of potassium carbonate and heated in the microwave oven to 150° C. for 3 h. The mixture is diluted with water and then extracted with ethyl acetate. The organic layers are washed with brine and dried over sodium sulfate. The solvent is evaporated and the resulting residue is dissolved in 5 ml TFA. 54 mg (0.44 mmol) thioanisole is added and the mixture is stirred over night. The solvent is evaporated, the resulting residue is dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layers are dried over sodium sulfate, the solvent is evaporated and the resulting residue is purified by preparative HPLC. 90 mg (46%) of the desired product are obtained

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layers are washed with brine
  3. dry with materialdried over sodium sulfate
  4. customThe solvent is evaporated
  5. dissolutionthe resulting residue is dissolved in 5 ml TFA
  6. customThe solvent is evaporated
  7. dissolutionthe resulting residue is dissolved in ethyl acetate
  8. washwashed with sat. NaHCO3 and brine
  9. dry with materialThe organic layers are dried over sodium sulfate
  10. customthe solvent is evaporated
  11. customthe resulting residue is purified by preparative HPLC