反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 2-(4-acetoxy-3,5-di-tert.- butylbenzylidene)-3,4-dihydro-3-oxo-4-(1H-tetrazol-5-ylmethyl)2H-1,4-benzothiazine (compound No. 8-1, 0.19 g) in ethanol (10 ml), potassium hydroxide (0.58 g) dissolved in water (10 ml) was added. The mixture was refluxed over night. 6N hydrochloric acid was added to the mixture to acidify it. The mixture was concentrated in vacuo and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo. The oily residue was purified by silica gel column chromatography to give the titled compound. The physical property of the compound obtained above was the same as the compound (No. 2-1) prepared in Example 2.
WORKUP
后处理
- additionwas added
- temperatureThe mixture was refluxed over night
- concentrationThe mixture was concentrated in vacuo
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customThe oily residue was purified by silica gel column chromatography