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(2-Methoxyethyl)urea → 1-(3-(4-fluorophenyl)-1H-pyrazolo[4,3-c]pyridin-6-yl)-3-(2-methoxyethyl)urea

HRID 571428
ノート
印刷プレビュー

反応式

HRID 571428 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]2[C:8]([C:11]3[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=3)=[N:9][NH:10][C:4]=2[CH:3]=1.[CH3:18][O:19][CH2:20][CH2:21][NH:22][C:23]([NH2:25])=[O:24].CC(C)([O-])C.[K+]>C1COCC1.CC(C1C=C(C(C)C)C(C2C(P(C3CCCCC3)C3CCCCC3)=C(OC)C=CC=2OC)=C(C(C)C)C=1)C.C1C=[C-]C(CCN)=CC=1.Cl[Pd+]>[F:17][C:14]1[CH:15]=[CH:16][C:11]([C:8]2[C:5]3[CH:6]=[N:7][C:2]([NH:25][C:23]([NH:22][CH2:21][CH2:20][O:19][CH3:18])=[O:24])=[CH:3][C:4]=3[NH:10][N:9]=2)=[CH:12][CH:13]=1
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

6

反応物 3

HCID 186068(2-Methoxyethyl)ureaHCID 23665647Potassium tert-butoxideHCID 768471656-Chloro-3-(4-fluorophenyl)-1H-pyrazolo[4,3-c]pyridine

生成物 1

HCID 895258561-(3-(4-fluorophenyl)-1H-pyrazolo[4,3-c]pyridin-6-yl)-3-(2-methoxyethyl)urea収率 41.2%

試薬・触媒・溶媒 2

HCID 25112666BrettPhos Palladacycle
触媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
60 °C

実験手順

6-Chloro-3-(4-fluorophenyl)-1H-pyrazolo[4,3-c]pyridine (433 mg, 1.748 mmol), 1-(2-methoxyethyl)urea (313 mg, 2.65 mmol) and chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-i-propyl-1,1′-biphenyl][2-(2-aminoethyl)phenyl]palladium(II) (97 mg, 0.121 mmol) were taken up in THF (10.5 mL) in a 20 mL microwave vial. 1 M potassium t-butoxide in THF (5.25 mL, 5.25 mmol) was added and the vial was evacuated and back-filled with N2 (x3). The reaction mixture was stirred at 60° C. for 18 hours. Room temperature was attained and the mixture filtered through Celite, eluting with MeOH. The filtrate was concentrated in vacuo and the residue purified by MPLC (0-10% MeOH-EtOAc). The product was then triturated in EtOH to give 1-(3-(4-fluorophenyl)-1H-pyrazolo[4,3-c]pyridin-6-yl)-3-(2-methoxyethyl)urea (237 mg, 0.720 mmol, 41.2% yield). MS ESI calc'd. for C16H17FN5O2 [M+H]+ 330, found 330. 1H NMR (600 MHz, DMSO-d6) δ 13.21 (s, 1H), 9.15 (s, 1H), 9.04 (s, 1H), 8.07-8.04 (m, 2H), 7.72 (s, 1H), 7.35-7.31 (m, 3H), 3.39 (t, J=5.5 Hz, 2H), 3.32-3.29 (m, 2H), 3.27 (s, 3H).

後処理

  1. customthe vial was evacuated
  2. additionback-filled with N2 (x3)
  3. customRoom temperature
  4. filtrationthe mixture filtered through Celite
  5. washeluting with MeOH
  6. concentrationThe filtrate was concentrated in vacuo
  7. customthe residue purified by MPLC (0-10% MeOH-EtOAc)
  8. customThe product was then triturated in EtOH

出典と根拠

ORDレコード
ord-40cf110bfb3f4b6891eee6fabd402daf
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09023865B2

反応ノート

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