* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With ammonium hydroxide; In acetonitrile; at 0 - 40℃;
C. Preparation of a Compound of Formula (3) in which R4 is CI, R6 and R7 are H2> and X is F To 2A^trifluoiopyrimidine (10 g, 75 mmol) in acetonitrile (100 mL) cooled to 0C is added cone NH OH (50 mL) in three portions. Remove the cooling bath and allow to stir at room temperature for 6 h followed by heating at 40CC overnight. Remove the solvent in vacuo to give 2,4^iamino~6~fluoropyiisnidine. MeOH EtOH (250 mL, 1:1) is added to the 2,4~diannno-6~ uoiOpyrimidine and the mixture is cooled with an ice bath. NCS (13 g, 97 mmol) was added in portions. The ice bath was removed and the mixture stirred for 6 h, followed by heating to 50C overnight. Approximately 75 mL of the solvent is removed in vacuo and the reaction vessel is cooled to -10C. The solid is collected by filtration and added to water (100 mL) and stirred. The solid is collected by filtration and added to 0.1M NaOH (1 0 mL) and stirred. The solid is collected by filtration to give 2,4-diamino-5~chloro~ 6-flixoropyrimidine.
With N-chloro-succinimide; In methanol; ethanol; at 50℃;Cooling with ice;
Example 3, Preparation of a Compound of Formula (3) C. Preparation of a Compound of Formula (3) in which R4 is CI, R6 and R7 are H2> and X is F To 2A^trifluoiopyrimidine (10 g, 75 mmol) in acetonitrile (100 mL) cooled to 0C is added cone NH OH (50 mL) in three portions. Remove the cooling bath and allow to stir at room temperature for 6 h followed by heating at 40CC overnight. Remove the solvent in vacuo to give 2,4^iamino~6~fluoropyiisnidine. MeOH EtOH (250 mL, 1:1) is added to the 2,4~diannno-6~ uoiOpyrimidine and the mixture is cooled with an ice bath. NCS (13 g, 97 mmol) was added in portions. The ice bath was removed and the mixture stirred for 6 h, followed by heating to 50C overnight. Approximately 75 mL of the solvent is removed in vacuo and the reaction vessel is cooled to -10C. The solid is collected by filtration and added to water (100 mL) and stirred. The solid is collected by filtration and added to 0.1M NaOH (1 0 mL) and stirred. The solid is collected by filtration to give 2,4-diamino-5~chloro~ 6-flixoropyrimidine.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
