HRID227721

反应详情

EQUATION

反应方程式

HRID 227721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product of Step (a) (10.0 g, 41.3 mmol, 1.00 equiv) was suspended in EtOH (120 mL). SnCl2.H2O (46.6 g, 206 mmol, 5.00 equiv) was added and the mixture was refluxed for 18 hours. The reaction mixture was concentrated en vacuo and water was added to the residue. The mixture was basified to pH 8 with satd. NaHCO3 and extracted with EtOAc (3×). The combined organic extracts were washed with satd. NaCl, dried over MgSO4, filtered and concentrated en vacuo. 8.10 g (92%) of the title compound was iolated as a purple solid.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 18 hours
  2. concentrationThe reaction mixture was concentrated en vacuo and water
  3. additionwas added to the residue
  4. extractionNaHCO3 and extracted with EtOAc (3×)
  5. washThe combined organic extracts were washed with satd
  6. dry with materialNaCl, dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated en vacuo