홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

3'-(1-Methyl-3-nitro-2-oxo-1,2-dihydropyridin-4-ylamino)biphenyl-2-carbonitrile → 3'-(3-Amino-1-methyl-2-oxo-1,2-dihydropyridin-4-ylamino)biphenyl-2-carbonitrile

HRID 2180032
노트
인쇄 미리보기

반응식

HRID 2180032 반응식
[CH3:1][N:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:10]=[C:11]([C:15]3[C:16]([C:21]#[N:22])=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:12]=[CH:13][CH:14]=2)=[C:4]([N+:23]([O-])=O)[C:3]1=[O:26]>C(OCC)(=O)C.C(O)C.[Pt]=O>[NH2:23][C:4]1[C:3](=[O:26])[N:2]([CH3:1])[CH:7]=[CH:6][C:5]=1[NH:8][C:9]1[CH:10]=[C:11]([C:15]2[C:16]([C:21]#[N:22])=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:12]=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 865933593'-(1-Methyl-3-nitro-2-oxo-1,2-dihydropyridin-4-ylamino)biphenyl-2-carbonitrile

생성물 1

HCID 697322603'-(3-Amino-1-methyl-2-oxo-1,2-dihydropyridin-4-ylamino)biphenyl-2-carbonitrile

시약·촉매·용매 3

HCID 82844Platinum oxide (PtO)촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

3′-(1-Methyl-3-nitro-2-oxo-1,2-dihydropyridin-4-ylamino)biphenyl-2-carbonitrile (0.11 g, 0.32 mmol) was suspended in ethyl acetate (10 ml) and ethanol (10 ml), platinum oxide (7.3 mg, 0.03 mmol) added and the mixture hydrogenated at 45 psi on a Parr hydrogenator for 2 h. The catalyst was filtered off through a glass fibre filter paper and the filtrate evaporated to give 3′-(3-amino-1-methyl-2-oxo-1,2-dihydropyridin-4-ylamino)biphenyl-2-carbonitrile as an orange oil. The oil was dissolved in formic acid (4 ml) and heated at 95° C. for 24 h. The mixture was allowed to cool to ambient temperature and evaporated. The residue was made basic by the addition of concentrated ammonia solution, then diluted with water (100 ml) and extracted with dichloromethane (2×100 ml). The combined organic layer was washed with brine (50 ml), dried over anhydrous sodium sulfate, filtered and evaporated to give a brown oil. The oil was purified by flash column chromatography on silica eluting with dichloromethane (+1% concentrated ammonia) on a gradient of methanol (2-4%). Collecting appropriate fractions, followed by trituration with diethyl ether (5 ml), gave 3′-(5-methyl-4-oxo-4,5-dihydroimidazo[4,5-c]pyridin-1-yl)biphenyl-2-carbonitrile (64 mg, 61%) as a white solid: δH (400 MHz, CDCl3) 3.69 (3H, s), 6.66 (1H, d, J 7), 7.24 (2H, m), 7.52-7.58 (2H, m), 7.65-7.67 (2H, m), 7.69-7.74 (2H, m), 7.84 (1H, dd, J 8 and 1), 7.99 (1H, s); m/z (ES+) 327 (M++H).

후처리

  1. filtrationThe catalyst was filtered off through a glass fibre
  2. filtrationfilter paper
  3. customthe filtrate evaporated

출처 및 근거

ORD 기록
ord-d401791faeb1420abbde22b6d90da4c7
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06887885B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트