反应详情

温度

2.5 °C

(189 mg) of 31-trimethyl silyl-42-ester of rapamycin with 5-methyl-2,2-diphenyl-1,3-dioxane-5-carboxylic acid [IId10] was dissolved in 2.8 ml THF and cooled to 0-5° C. Into the reaction mass 0.52 ml 2N sulphuric acid was added and stirred at 25-30° C. for 24 hrs. Then 2 ml THF and 0.52 ml 2 N sulphuric acid was added and stirred at 25-30° C. for 76 hrs. It was then concentrated on rotavapour, residue was dissolved in 2 ml ethyl acetate, and 2-3 drop perchloric acid (HClO4) diluted with 1 ml water was added. The reaction mixture was stirred at 25-30° C. for 24 hrs and reaction mass was dumped into water, and extracted with ethyl acetate. The layers were separated and washed the organic layer with 10% sodium bicarbonate solution and then water. It was dried over sodium sulfate, concentrated on rotavapor to obtain yellow colored oily compound.

1. stirringstirred at 25-30° C. for 76 hrs
2. concentrationIt was then concentrated on rotavapour, residue
3. dissolutionwas dissolved in 2 ml ethyl acetate
4. addition2-3 drop perchloric acid (HClO4) diluted with 1 ml water
5. additionwas added
6. stirringThe reaction mixture was stirred at 25-30° C. for 24 hrs
7. customreaction mass
8. extractionextracted with ethyl acetate
9. customThe layers were separated
10. washwashed the organic layer with 10% sodium bicarbonate solution
11. dry with materialIt was dried over sodium sulfate
12. concentrationconcentrated on rotavapor
13. customto obtain yellow colored oily compound