반응 #58366

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ammonia

2-[(2-aminoethyl)amino]-8-(2,6-difluorophenyl)-4-(2-methylphenyl)pyrido[2,3-d]pyrimidin-7(8H)-one

diphenyl cyanocarbonimidate

→

title compound

수율 59.0%

N-Cyano-N′-(2-{[8-(2,6-difluorophenyl)-4-(2-methylphenyl)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-2-yl]amino}ethyl) guanidine

수율 59.0%

용매

isopropanol

isopropanol

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후처리

1. 1
   workup.STIRRINGthe mixture stirred at about 20° C. for about 3 days
2. 2
   기타The solvent was evaporated
3. 3
   workup.DISSOLUTIONthe residue redissolved in 2M ammonia in isopropanol (2 mL)
4. 4
   기타The mixture was irradiated with microwave at about 60° C. for about 40 min
5. 5
   workup.WAITThe mixture was stored in a sealed tube for 7 days
6. 6
   기타The solvent was evaporated
7. 7
   기타the crude product was purified

실험 절차

To a solution of 2-[(2-aminoethyl)amino]-8-(2,6-difluorophenyl)-4-(2-methylphenyl)pyrido[2,3-d]pyrimidin-7(8H)-one (20 mg, 0.050 mmol) in isopropanol (2 mL) was added diphenyl cyanocarbonimidate (12 mg, 0.050 mmol) and the mixture was stirred for about 1 hour at about 20° C. A 2M solution of ammonia in isopropanol (2 ml) was added and the mixture stirred at about 20° C. for about 3 days. The solvent was evaporated and the residue redissolved in 2M ammonia in isopropanol (2 mL). The mixture was irradiated with microwave at about 60° C. for about 40 min. The mixture was stored in a sealed tube for 7 days. The solvent was evaporated and the crude product was purified to give the title compound (14 mg, 59%). LC-MS m/z 475 (M+H)+, 2.93 min (ret time).

출처