Reaktion #2313203

Reaktionsgleichung

diethyl N-[4-(1-(tetrahydropyr-2-yloxy)-3-(4-hydroxy-6-pivaloylaminopyrrolo-[2,3-d]pyrimidin-3-yl)prop-2-yl)benzoyl]glutamate

sodium carbonate

methanol

→

diethyl N-[4-{1-hydroxy-3-(4-hydroxy-6-pivaloylaminopyrrolo[2,3-d]-pyrimidin-3-yl)prop-2-yl}benzoyl]glutamate

Lösungsmittel

hydrogen chloride

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeremoved by evaporation under reduced pressure
2. 2
   workup.ADDITIONOne hundred milliliters of methylene chloride are added
3. 3
   Waschenthe solution is washed twice with 20 ml of water
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   Einengenconcentrated
6. 6
   SonstigeThe residue is triturated with 1:2 ethyl acetate and ether
7. 7
   Filtrationfiltered
8. 8
   Sonstigedried

Vorschrift

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.

Quelle