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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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6-Methylpyridine-2-carboxylic acid → HCID 58268015, 화합물

HRID 1615985
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HRID 1615985 반응식
[CH3:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[CH:5]=[CH:4][CH:3]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[Br:44][C:45]1[CH:46]=[C:47]([NH2:55])[C:48]2[CH:49]=[N:50][N:51]([CH3:54])[C:52]=2[CH:53]=1>CN(C=O)C.O>[Br:44][C:45]1[CH:53]=[C:52]2[C:48]([CH:49]=[N:50][N:51]2[CH3:54])=[C:47]([NH:55][C:8]([C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=2)=[O:10])[CH:46]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 702826-Methylpyridine-2-carboxylic acidHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 582557716-Bromo-1-methyl-1h-indazol-4-amine

생성물 1

HCID 58268015HCID 58268015, 화합물수율 64.4%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

6-Methyl-2-pyridinecarboxylic acid (74 mg, 0.54 mmol) and HATU (250 mg, 0.65 mmol) were dissolved in DMF (4 ml) and then DIPEA (0.23 ml) was then added. The mixture was stirred under nitrogen for 30 min. 6-bromo-1-methyl-1H-indazol-4-amine (135 mg, 0.60 mmol) was then added and stirring was continued under nitrogen overnight. Addition of water was followed by extraction of the resultant mixture with DCM (2×10 ml). The organics were combined and concentrated in vacuo then the residue was purified by chromatography on silica eluting with a gradient of 0-100% ethyl acetate in DCM. Fractions containing desired material were combined and concentrated in vacuo to afford the title compound (120 mg).

후처리

  1. stirringstirring
  2. waitwas continued under nitrogen overnight
  3. extractionwas followed by extraction of the resultant mixture with DCM (2×10 ml)
  4. concentrationconcentrated in vacuo
  5. customthe residue was purified by chromatography on silica eluting with a gradient of 0-100% ethyl acetate in DCM
  6. additionFractions containing desired material
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-111ce5fd2ca44b33bdefc8847ceb860a
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765743B2

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