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4-Methylmorpholine → N-(indazol-5-yl) N2-(4-pyridylmethyl)-anthranilic acid amide

HRID 1244293
ノート
印刷プレビュー

反応式

HRID 1244293 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][NH:8][C:9]2[C:10](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:11]([OH:13])=O)=[CH:3][CH:2]=1.[NH2:18][C:19]1[CH:20]=[C:21]2[C:25](=[CH:26][CH:27]=1)[NH:24][N:23]=[CH:22]2.CN1CCOCC1.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.C(=O)(O)[O-].[Na+]>CN(C)C=O>[NH:24]1[C:25]2[C:21](=[CH:20][C:19]([NH:18][C:11](=[O:13])[C:10]3[C:9](=[CH:17][CH:16]=[CH:15][CH:14]=3)[NH:8][CH2:7][C:4]3[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=3)=[CH:27][CH:26]=2)[CH:22]=[N:23]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 79724-MethylmorpholineHCID 880121H-Indazol-5-amineHCID 516892Sodium BicarbonateHCID 3239010HCID 3239010、化合物HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

生成物 1

HCID 69590332
N-(indazol-5-yl) N2-(4-pyridylmethyl)-anthranilic acid amide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

228 mg of N-(4-pyridylmethyl)-anthranilic acid is introduced into 10 ml of dimethylformamide under argon and in a moisture-free environment. 266 mg of 5-aminoindazole, 0.27 ml of methylmorpholine and 456 mg of O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HATU) are added. The mixture is then stirred for 4 hours at room temperature. It is then mixed with dilute sodium bicarbonate solution and extracted three times with ethyl acetate. The combined organic phases are washed with water, dried, filtered and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel with ethyl acetate as an eluant.

後処理

  1. extractionextracted three times with ethyl acetate
  2. washThe combined organic phases are washed with water
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated by evaporation in a vacuum
  6. customThe residue is chromatographed on silica gel with ethyl acetate as an eluant

出典と根拠

ORDレコード
ord-e9be399065004956a7937ac19f607d89
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07122547B1

反応ノート

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