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

Potassium Carbonate → 6-Methyl-5-(1-methyl-1H-pyrazol-5-yl)-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylic acid

HRID 1517470
노트
인쇄 미리보기

반응식

HRID 1517470 반응식
C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.C(=O)([O-])[O-].[K+].[K+].[CH3:36][N:37]1[C:41](B2OC(C)(C)C(C)(C)O2)=[CH:40][CH:39]=[N:38]1.I[C:52]1[CH:53]=[C:54]([C:70]([OH:72])=[O:71])[C:55](=[O:69])[N:56]([C:59]2[CH:64]=[CH:63][CH:62]=[C:61]([C:65]([F:68])([F:67])[F:66])[CH:60]=2)[C:57]=1[CH3:58]>O.C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:58][C:57]1[N:56]([C:59]2[CH:64]=[CH:63][CH:62]=[C:61]([C:65]([F:67])([F:68])[F:66])[CH:60]=2)[C:55](=[O:69])[C:54]([C:70]([OH:72])=[O:71])=[CH:53][C:52]=1[C:41]1[N:37]([CH3:36])[N:38]=[CH:39][CH:40]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 49129081-methyl-5-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazoleHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 582180465-Iodo-6-methyl-2-oxo-1-(3-(trifluoromethyl)phenyl)-1,2-dihydropyridine-3-carboxylic acid

생성물 1

HCID 594558756-Methyl-5-(1-methyl-1H-pyrazol-5-yl)-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylic acid
수율 77%

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 962Water용매HCID 6342Acetonitrile용매2회

반응 조건

온도
50 °C

실험 절차

Acetonitrile (30.3 L, 3 rel vol) was charged, followed by palladium(II) acetate (260 g, 0.05 mol eq) and 2-dicyclohexylphosphino-2′,6′-dimethoxy-1,1′-biphenyl (980 g, 0.1 mol eq). The mixture was stirred for 15 minutes. A solution of potassium carbonate (10.0 kg, 3.0 mol eq) in water (60.6 L, 6 rel vol) was added to the reaction. 1-Methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (31.8% w/w, 20.3 kg, 1.3 mol eq) as a solution in acetonitrile was added, followed by 5-iodo-6-methyl-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylic acid (10.1 kg, 1 mol eq, limiting reagent). The reaction mixture was heated to reflux and stirred until the reaction was complete as judged by HPLC analysis. The reaction mixture was cooled and filtered. The cake was washed with acetonitrile (10.1 L, 1 rel vol) and the cake discarded. The filtrate was heated to 50° C. 6 M Hydrochloric acid (60.6 L, 6 rel vol) was added carefully to the reaction. The reaction mixture was stirred at 50° C. for 60 minutes, cooled to 5° C. and stirred overnight. The solid was collected by filtration, washed twice with water (2×20.2 L, 2×2 rel vol) and with cold (around 5° C.) acetonitrile (10.1 L, 1 rel vol). The solid was dried to constant weight to yield the title compound (8.1 kg, 21.5 mol, 77%); 1H NMR (d6-DMSO): δ 1.87 (s, 3H); 3.73 (s, 3H); 6.35-6.37 (m, 1H); 7.54-7.55 (m, 1H); 7.83-7.91 (m, 2H); 7.95-7.97 (m, 1H); 8.07 (s, 1H); 8.25 (s, 1H); 13.80 (s, 1H); LCMS: m/z 378.3 (MH+).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux
  3. stirringstirred until the reaction
  4. temperatureThe reaction mixture was cooled
  5. filtrationfiltered
  6. washThe cake was washed with acetonitrile (10.1 L, 1 rel vol)
  7. addition6 M Hydrochloric acid (60.6 L, 6 rel vol) was added carefully to the reaction
  8. stirringThe reaction mixture was stirred at 50° C. for 60 minutes
  9. temperaturecooled to 5° C.
  10. stirringstirred overnight
  11. filtrationThe solid was collected by filtration
  12. washwashed twice with water (2×20.2 L, 2×2 rel vol) and with cold (around 5° C.) acetonitrile (10.1 L, 1 rel vol)
  13. customThe solid was dried to constant weight

출처 및 근거

ORD 기록
ord-7a111f5d4a0844e4ab67840359fc0512
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232296B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트