Diisopropylethylamine → 2-[(S)-1-phenylethylamino]-4-[5-(pyridin-4-yl)aminobenzimidazol-1-yl]pyrimidine

온도

100 °C

2-[(S)-1-phenylethylamino]-4-[5-aminobenzimidazol-1-yl]pyrimidine (49.8 mg) was dissolved in DMF (2 mL). Diisopropylethylamine (79 μL) and 4-bromopyridine hydrochloride (43.2 mg) were added, and the mixture left heating overnight at 100° C. After 17 h added more diisopropylethylamine (79 μL) and 4-bromopyridine hydrochloride (40.2 mg) and continued heating at 100° C. for another 24 h. The volatiles were removed in vacuo and the residue purified on silica gel (2-5%(2M NH3 in MeOH)/CH2Cl2) to yield 5.0 mg of impure product that was purified by HPLC (Zorbax Rx-SIL, 60:40 hexanes:ethanol) to yield 3.0 mg of the title compound. Mass spectrum (ESI) 408.4 (M+1).

1. waitthe mixture left
2. temperaturecontinued heating at 100° C. for another 24 h
3. customThe volatiles were removed in vacuo
4. customthe residue purified on silica gel (2-5%(2M NH3 in MeOH)/CH2Cl2)

ORD 기록

ord-a1c10b40483c4f658deebc2f605d02ee

출처 데이터셋

uspto-grants-2002_12

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06498165B1