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Water → N-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-N-{[3'-formyl-5-(methyloxy)-3-biphenylyl]methyl}-1,3-benzenedicarboxamide

HRID 564535
ノート
印刷プレビュー

反応式

HRID 564535 の反応式
BrC1C=C(C[NH:11][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([NH:22][CH2:23][C:24]3[C:25]([NH:37][CH:38]4[CH2:43][CH2:42][O:41][CH2:40][CH2:39]4)=[C:26]4[CH:34]=[N:33][N:32]([CH2:35][CH3:36])[C:27]4=[N:28][C:29]=3[CH2:30][CH3:31])=[O:21])[CH:15]=2)=[O:13])C=C(OC)C=1.[CH:44]([C:46]1[CH:47]=[C:48](B(O)O)[CH:49]=[CH:50][CH:51]=1)=[O:45].[C:55]([O-:58])([O-])=O.[Na+].[Na+].O>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:35]([N:32]1[C:27]2=[N:28][C:29]([CH2:30][CH3:31])=[C:24]([CH2:23][N:22]([CH2:12][C:14]3[CH:15]=[C:16]([C:48]4[CH:49]=[CH:50][CH:51]=[C:46]([CH:44]=[O:45])[CH:47]=4)[CH:17]=[C:18]([O:58][CH3:55])[CH:19]=3)[C:20]([C:16]3[CH:17]=[CH:18][CH:19]=[C:14]([C:12]([NH2:11])=[O:13])[CH:15]=3)=[O:21])[C:25]([NH:37][CH:38]3[CH2:43][CH2:42][O:41][CH2:40][CH2:39]3)=[C:26]2[CH:34]=[N:33]1)[CH3:36]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 27343563-Formylphenylboronic acidHCID 57813286N-{[3-bromo-5-(methyloxy)phenyl]methyl}-N'-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-1,3-benzenedicarboxamide

生成物 1

HCID 86633199
N-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-N-{[3'-formyl-5-(methyloxy)-3-biphenylyl]methyl}-1,3-benzenedicarboxamide
収率 169.7%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
150 °C

実験手順

A mixture of N-{[3-bromo-5-(methyloxy)phenyl]methyl}-N′-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-1,3-benzenedicarboxamide (782 mg, 1.20 mmol), 3-formylphenyl boronic acid (234 mg, 1.57 mmol), Na2CO3 (383 mg, 3.61 mmol), Pd(PPh3)4 (69.6 mg, 0.06 mmol), and water (3 mL) in dioxane (9 mL) was degassed for 5 min. This mixture was then heated under microwave for 30 min at 150° C. It was quenched with water and then extracted with ethyl acetate twice. The combined organic layers were washed with water and brine. The organic layer was filtered though a 0.45 μM filter and then concentrated to give a crude residue. It was then purified with Combi Flash chromatography eluting with 0 to 10% MeOH in DCM. The product fractions were combined and concentrated under vacuum to give N-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-N-{[3′-formyl-5-(methyloxy)-3-biphenylyl]methyl}-1,3-benzenedicarboxamide as a solid (687 mg, 85%). LC-MS m/z 676 (M+H)+.

後処理

  1. customwas degassed for 5 min
  2. customIt was quenched with water
  3. extractionextracted with ethyl acetate twice
  4. washThe combined organic layers were washed with water and brine
  5. filtrationThe organic layer was filtered though a 0.45 μM
  6. filtrationfilter
  7. concentrationconcentrated
  8. customto give a crude residue
  9. customIt was then purified with Combi Flash chromatography
  10. washeluting with 0 to 10% MeOH in DCM
  11. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-aee06529333f4a9dbfd95757eeda0445
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08067408B2

反応ノート

読み込み中…

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