反应详情

The solution of 0.94 g of diethyl N-[4-(1-(tetrahydropyr-2-yloxy)-3-(4-hydroxy-6-pivaloylaminopyrrolo-[2,3-d]pyrimidin-3-yl)prop-2-yl)benzoyl]glutamate in 40 ml of 0.1N methanolic hydrogen chloride is stirred at ambient temperatures for 2 hours. The reaction mixture is neutralized with a solution of 205 mg of sodium carbonate in 10 ml of water and most of methanol removed by evaporation under reduced pressure. One hundred milliliters of methylene chloride are added and the solution is washed twice with 20 ml of water, dried over anhydrous magnesium sulfate, and concentrated. The residue is triturated with 1:2 ethyl acetate and ether, filtered, and dried to give diethyl N-[4-{1-hydroxy-3-(4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]-pyrimidin-3-yl)prop-2-yl}benzoyl]glutamate.

1. customremoved by evaporation under reduced pressure
2. additionOne hundred milliliters of methylene chloride are added
3. washthe solution is washed twice with 20 ml of water
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customThe residue is triturated with 1:2 ethyl acetate and ether
7. filtrationfiltered
8. customdried