Cesium fluoride → (S)-4-(N-Methylsulfamoyl)phenyl 4-amino-6-((1-(5-methyl-4-oxo-3-phenyl-3,4-dihydropyrrolo[2,1-f][1,2,4]triazin-2-yl)ethyl)amino)pyrimidine-5-carboxylate

温度

80 °C

(S)-2-(1-Aminoethyl)-5-methyl-3-phenylpyrrolo[2,1-f][1,2,4]triazin-4(3H)-one (81 mg, 0.27 mmol), 4-(N-methylsulfamoyl)phenyl 4-amino-6-chloropyrimidine-5-carboxylate (135 mg, 0.39 mmol), DIEA (344 μl, 1.97 mmol) and cesium fluoride (150 mg, 0.99 mmol) were suspended in tert-butanol (10 ml) and the mixture was heated at 80° C. in a sealed tube for 24 h. The solvent was evaporated under reduced pressure and the reaction mixture was diluted with ethyl acetate and washed with saturated ammonium chloride solution and brine. After evaporation of the solvent, the residue was purified by reverse phase chromatography using SP1® Purification System to give 27 mg (14% yield) as a solid. Purity 99%.

1. customThe solvent was evaporated under reduced pressure
2. additionthe reaction mixture was diluted with ethyl acetate
3. washwashed with saturated ammonium chloride solution and brine
4. customAfter evaporation of the solvent
5. customthe residue was purified by reverse phase chromatography
6. customSP1® Purification System
7. customto give 27 mg (14% yield) as a solid

ORDレコード

ord-1b9d5e97bd284e47993e224d8da9ddbf

出典データセット

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09388189B2