HRID524414

反应详情

EQUATION

反应方程式

HRID 524414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thiourea (0.672 g, 8.835 mmol) was taken in ethanol (30 mL). To this stirred solution was added 3-Bromo-4-oxo-cyclohexane carboxylic acid ethyl ester (2.2 g, 8.835 mmol). The reaction was refluxed for 2 hrs. The reaction mixture was allowed to cool to room temperature and ethanol was evaporated under reduced pressure, the residue was partitioned between water and ethyl acetate. The water layer was collected and basified using sat. sodium bicarbonate solution, extracted with ethyl acetate, the organic layer was washed with brine, dried over anhydrous sodium sulfate filtered and concentrated under reduced pressure to afford 2-Amino-4,5,6,7-tetrahydro-benzothiazole-6-carboxylic acid ethyl ester (1.6 g)

WORKUP

后处理

  1. temperatureThe reaction was refluxed for 2 hrs
  2. customethanol was evaporated under reduced pressure
  3. customthe residue was partitioned between water and ethyl acetate
  4. customThe water layer was collected
  5. extractionextracted with ethyl acetate
  6. washthe organic layer was washed with brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure