HRID1158914
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 the stirred solution of ethyl2,3-dihydropyrazolo[5,1-b][1,3]oxazole-6-carboxylate (5.47 g, 35 mmol) of in 100 ml of THF was added 1.05 g of lithium borohydride and 1.54 g of methanol. The solution was heated at 40 C for 2.5 hour. The reaction was quenched by 1N HCl, and adjusted to pH 1.3 and stirred at room temperature for 1 hour. The reaction mixture was adjusted pH to 8 with k2CO3. The reaction mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4, and concentrated to an oil and column chromatographed to give 2.68 g of the desired product (65%).
WORKUP
后处理
- temperatureThe solution was heated at 40 C for 2.5 hour
- customThe reaction was quenched by 1N HCl
- extractionThe reaction mixture was extracted with ethyl acetate
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated to an oil and column
- customchromatographed