HRID33393

反应详情

EQUATION

反应方程式

HRID 33393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.7 g (8.7 mmol) 5-methoxy-3-methyl-1-(3-methyl-3-nitro-butyl)-1,3-dihydro-benzimidazol-2-one and 9.93 g (44.0 mmol) SnCl2 2H2O in 200 mL ethanol are refluxed for 3 hours. The reaction mixture is evaporated down, combined with sodium carbonate solution and filtered. The filtrate is extracted with ethyl acetate and the combined organic phases are washed with water, dried and freed from the solvent. The residue is dissolved in ethanol and the solution is combined with ethereal hydrochloric acid. After the solvent has been distilled off the solid remaining is stirred with diisopropylether.

WORKUP

后处理

  1. customThe reaction mixture is evaporated down
  2. filtrationfiltered
  3. extractionThe filtrate is extracted with ethyl acetate
  4. washthe combined organic phases are washed with water
  5. customdried
  6. dissolutionThe residue is dissolved in ethanol
  7. distillationAfter the solvent has been distilled off the solid