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Dichloromethane → 5-(1-methyl-1H-pyrazol-4-yl)-3-phenyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-c]pyridine

HRID 1774973
ノート
印刷プレビュー

反応式

HRID 1774973 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)=[N:9][N:8]([CH:17]3[CH2:22][CH2:21][CH2:20][CH2:19][O:18]3)[C:5]2=[CH:6][N:7]=1.[CH3:23][N:24]1[CH:28]=[C:27](B2OC(C)(C)C(C)(C)O2)[CH:26]=[N:25]1.C([O-])(=O)C.[K+].C(=O)([O-])[O-].[Na+].[Na+].ClCCl>C1(P([C-]2C=CC=C2)C2C=CC=CC=2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2].Cl[Pd]Cl.O.C(#N)C>[CH3:23][N:24]1[CH:28]=[C:27]([C:2]2[CH:3]=[C:4]3[C:10]([C:11]4[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=4)=[N:9][N:8]([CH:17]4[CH2:22][CH2:21][CH2:20][CH2:19][O:18]4)[C:5]3=[CH:6][N:7]=2)[CH:26]=[N:25]1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 27739871-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazoleHCID 866766845-bromo-3-phenyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-c]pyridine

生成物 1

HCID 71253501
5-(1-methyl-1H-pyrazol-4-yl)-3-phenyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-c]pyridine
収率 68.1%

試薬・触媒・溶媒 4

HCID 24290Palladium Chloride触媒HCID 635956Ferrocene-1,1'-bis-(diphenylphosphine)触媒HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

In a microwave vial was charged with 5-bromo-3-phenyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-c]pyridine (500 mg, 1.39 mmol), 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (435.6 mg, 2.09 mmol), potassium acetate (205.5 mg, 2.09 mmol), sodium carbonate (221.9 mg, 2.09 mmol), and bis(diphenylphosphino)ferrocene]dichloropalladium (II), complexed with dichloromethane (1:1) (108.3 mg, 0.13 mmol). Degassed acetonitrile (10.5 mL) and water (2.6 mL) were added. Nitrogen was passed through the mixture for 15 minutes and the vial was capped. The reaction mixture was subjected to microwave irradiation at 125° C. for 25 min. The reaction mixture was filtered through a pad of Celite® and diluted with water and EtOAc. The organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude product was purified using flash chromatography (Si-PPC gradient elution, solvent: 60-100% ethyl acetate in heptanes, followed by 0-30% methanol in ethyl acetate) to give 5-(1-methyl-1H-pyrazol-4-yl)-3-phenyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-c]pyridine as a foam (340.0 mg, 67.8%). 1H NMR (400 MHz, CDCl3) δ 9.15 (s, 1H), 8.07-7.94 (m, 5H), 7.54 (t, J=7.6 Hz, 2H), 7.45 (t, J=7.4 Hz, 1H), 5.88 (dd, J=8.8, 2.2 Hz, 1H), 4.06 (dd, J=11.8, 4.0 Hz, 1H), 3.98 (s, 3H), 3.86-3.76 (m, 1H), 2.66-2.52 (m, 1H), 2.19 (d, J=10.8 Hz, 2H), 1.89-1.67 (m, 3H). LC/MS: m/z 378.3 [M+1]

後処理

  1. customthe vial was capped
  2. customirradiation at 125° C. for 25 min
  3. filtrationThe reaction mixture was filtered through a pad of Celite®
  4. additiondiluted with water and EtOAc
  5. washThe organic layer was washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe crude product was purified
  10. washflash chromatography (Si-PPC gradient elution, solvent: 60-100% ethyl acetate in heptanes, followed by 0-30% methanol in ethyl acetate)

出典と根拠

ORDレコード
ord-3591ee6d495c4390a898f84d50544102
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09260425B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート