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Urea → Pexmetinib

HRID 1665993
ノート
印刷プレビュー

反応式

HRID 1665993 の反応式
NC(N)=O.[C:5]([C:9]1[CH:13]=[C:12]([NH:14][C:15]([NH:17][CH2:18][C:19]2[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=2[O:26][C:27]2[CH:28]=[C:29]3[C:33](=[CH:34][CH:35]=2)[N:32]([CH2:36][CH:37]=[O:38])[N:31]=[CH:30]3)=[O:16])[N:11]([C:39]2[CH:44]=[CH:43][C:42]([CH3:45])=[CH:41][CH:40]=2)[N:10]=1)([CH3:8])([CH3:7])[CH3:6].[BH4-].[Na+]>CO>[C:5]([C:9]1[CH:13]=[C:12]([NH:14][C:15]([NH:17][CH2:18][C:19]2[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=2[O:26][C:27]2[CH:28]=[C:29]3[C:33](=[CH:34][CH:35]=2)[N:32]([CH2:36][CH2:37][OH:38])[N:31]=[CH:30]3)=[O:16])[N:11]([C:39]2[CH:44]=[CH:43][C:42]([CH3:45])=[CH:41][CH:40]=2)[N:10]=1)([CH3:8])([CH3:7])[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1176UreaHCID 4311764Sodium borohydrideHCID 575522811-(3-tert-Butyl-1-p-tolyl-1H-pyrazol-5-yl)-3-((5-fluoro-2-(1-(2-oxoethyl)-1H-indazol-5-yloxy)phenyl)methyl)urea

生成物 1

HCID 24765037Pexmetinib収率 55.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Preparation of 1-(3-tert-butyl-1-p-tolyl-1H-pyrazol-5-yl)-3-(5-fluoro-241-(2-hydroxyethyl)-1H-indazol-5-yloxy)benzyl)urea 72: 1-(3-tert-Butyl-1-p-tolyl-1H-pyrazol-5-yl)-3-((5-fluoro-2-(1-(2-oxoethyl)-1H-indazol-5-yloxy)phenyl)methyl)urea (2.179 g, 3.929 mmol) was suspended in MeOH (40 mL) and treated with sodium borohydride (0.7432 g, 19.64 mmol) portionwise at room temperature. The reaction mixture was stirred at room temperature until complete conversion of the starting material to product was observed by HPLC analysis. The reaction mixture was concentrated under reduced pressure and then diluted with saturated aqueous NH4Cl and extracted into dichloromethane. The organics were dried (MgSO4) and concentrated under reduced pressure to afford the crude material, which was purified by flash column chromatography (eluant 2-6% iPrOH/DCM) to provide 1.21 g (55%) of the desired compound. MS (APCI+) m/z 557 (M+1) was detected. 1H NMR (400 MHz, DMSO-d6) δ 8.29 (s, 1H), 7.97 (s, 1H), 7.68 (d, 1H, J=9.1 Hz), 7.35 (s, 1H), 6.85-7.4 (m, 8H), 6.24 (s, 1H), 4.87 (t, 1H, J=5.4 Hz), 4.43 (t, 1H, J=5.6 Hz), 4.28 (d, 1H, J=5.9 Hz), 3.80 (q, 1H, J=5.5 Hz), 2.35 (s, 3H), 1.25 (s, 9H).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additiondiluted with saturated aqueous NH4Cl
  3. extractionextracted into dichloromethane
  4. dry with materialThe organics were dried (MgSO4)
  5. concentrationconcentrated under reduced pressure
  6. customto afford the crude material, which
  7. customwas purified by flash column chromatography (eluant 2-6% iPrOH/DCM)

出典と根拠

ORDレコード
ord-0f989794d18b4ccdb14569ce6b2aa629
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039639B2

反応ノート

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