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Dimethylformamide → N-(5-(3-formyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-5-yl)pyridin-3-yl)pivalamide

HRID 589488
ノート
印刷プレビュー

反応式

HRID 589488 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:10]([CH:11]=[O:12])=[N:9][N:8]([C:13]([C:26]3[CH:31]=[CH:30][CH:29]=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[C:5]2=[N:6][CH:7]=1.B1(B2OC(C)(C)C(C)(C)O2)O[C:35](C)(C)[C:34]([CH3:40])([CH3:39])O1.CC([O-])=[O:52].[K+].Br[C:56]1[CH:57]=[C:58]2C(C(OC)=O)=NN[C:59]2=[N:60][CH:61]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C[N:78]([CH:80]=[O:81])C>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].O>[CH:11]([C:10]1[C:4]2[C:5](=[N:6][CH:7]=[C:2]([C:58]3[CH:57]=[C:56]([NH:78][C:80](=[O:81])[C:34]([CH3:40])([CH3:39])[CH3:35])[CH:61]=[N:60][CH:59]=3)[CH:3]=2)[N:8]([CH:13]2[CH2:26][CH2:31][CH2:30][CH2:29][O:52]2)[N:9]=1)=[O:12]
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

9

反応物 6

HCID 6228DimethylformamideHCID 62657Potassium Phosphate, TribasicHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 867010605-bromo-1-trityl-1H-pyrazolo[3,4-b]pyridine-3-carbaldehydeHCID 178499173HCID 178499173、化合物

生成物 1

HCID 86701079
N-(5-(3-formyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-5-yl)pyridin-3-yl)pivalamide
収率 68%

試薬・触媒・溶媒 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A solution of 5-bromo-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-carbaldehyde (XI) (436 mg, 1.4 mmol), bis(pinacolato)diboron (426 mg, 1.6 mmol), and KOAc (412 mg, 4.2 mmol) in dry DMF (20 ml) was purged with argon. PdCl2(dppf)2 (68 mg, 0.08 mmol) was added to the solution and purged again with argon. The solution was heated at 90° C. for 2 h under argon and cooled to the room temperature. N-(5-bromopyridin-3-yl)pivalamide (XVII) (358 mg, 1.4 mmol), potassium phosphate (446 mg, 2.1 mmol) and water (2 mL) was added to the solution and purged with argon. Pd(PPh3)4 was then added and the solution was again purged with the argon. The solution was heated at 90° C. for 4 h under argon. The solution was filtered through a bed of Celite and the solvent was distilled under vacuum. The crude product was suspended in water, sonicated briefly. The solids were filtered, dried under vacuum and purified by flash chromatography (100% DCM→3:97 MeOH:DCM) to get N-(5-(3-formyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-5-yl)pyridin-3-yl)pivalamide (LXV) as a brown solid (390 mg, 0.96 mmol, 68% yield). 1H NMR (DMSO-d6, 500 MHz) δ ppm 1.27 (s, 9H), 1.58-1.69 (m, 2H), 1.78-1.90 (m, 1H), 2.02-2.14 (m, 2H), 2.49-2.57 (m, 1H), 3.78 (dt, J=11 Hz, J=4 Hz, 1H), 3.94-4.03 (d, J=11 Hz, 1H), 6.25 (dd, J=10 Hz, J=2 Hz, 1H), 8.44 (t, J=2 Hz, 1H), 8.72 (dd, J=4 Hz, J=2 Hz, 2H), 8.98 (d, J=2 Hz, 1H), 9.09 (d, J=2 Hz, 1H), 9.60 (s, 1H), 10.21 (s, 1H); ESIMS found C22H25N5O3 m/z 408 (M+H).

後処理

  1. custompurged again with argon
  2. temperaturecooled to the room temperature
  3. custompurged with argon
  4. additionPd(PPh3)4 was then added
  5. customthe solution was again purged with the argon
  6. temperatureThe solution was heated at 90° C. for 4 h under argon
  7. filtrationThe solution was filtered through a bed of Celite
  8. distillationthe solvent was distilled under vacuum
  9. customsonicated briefly
  10. filtrationThe solids were filtered
  11. customdried under vacuum
  12. custompurified by flash chromatography (100% DCM→3:97 MeOH:DCM)

出典と根拠

ORDレコード
ord-d1451c3be6e14b30bf094bc919838de7
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09233104B2

反応ノート

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