HRID406966

反应详情

EQUATION

反应方程式

HRID 406966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionwas added
  2. extractionextracted by ethyl acetate
  3. customOrganic layer was separated
  4. washwash it with sodium bicarbonate solution
  5. customDried
  6. additionby adding sodium sulfate
  7. concentrationconcentrate it on rotavapour
  8. customto get colorless viscous oily product
  9. stirringstirred for 30 minute
  10. customWhite solid was precipitated
  11. filtrationwhich was filtered
  12. washwashed with n-hexane
  13. customto get white solid product