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
CONDITIONS
反应条件
- 温度
- 2.5 °C
PROCEDURE
实验过程
(160 mg) of 42-ester of rapamycin with 3-methyl-1,5-dioxaspiro[5.6]dodecane-3-carboxylic acid [IId6] was dissolved in 4 ml THF and was cooled it at 0-5° C. Subsequently, 0.5 ml 2N sulphuric acid was added and the reaction mass was stirred at 30-35° C. for 20 hrs. After completion of the reaction brine solution was added and extracted by ethyl acetate. Organic layer was separated and wash it with sodium bicarbonate solution and then by water. Dried by adding sodium sulfate and concentrate it on rotavapour to get colorless viscous oily product. Subsequently, n-hexane was added and stirred for 30 minute. White solid was precipitated, which was filtered, washed with n-hexane to get white solid product.
WORKUP
后处理
- additionwas added
- extractionextracted by ethyl acetate
- customOrganic layer was separated
- washwash it with sodium bicarbonate solution
- customDried
- additionby adding sodium sulfate
- concentrationconcentrate it on rotavapour
- customto get colorless viscous oily product
- stirringstirred for 30 minute
- customWhite solid was precipitated
- filtrationwhich was filtered
- washwashed with n-hexane
- customto get white solid product