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2-Methoxyethanol → 1-{5-tert-Butyl-2-[4-(2-methoxy-ethoxymethyl)-phenyl]-2H-pyrazol-3-yl}-3-[2-fluoro-4-(2-methyl-pyridin-4-yloxy)-phenyl]-urea

HRID 221910
ノート
印刷プレビュー

反応式

HRID 221910 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([NH:18][C:19]([NH:21][C:22]2[CH:27]=[CH:26][C:25]([O:28][C:29]3[CH:34]=[CH:33][N:32]=[C:31]([CH3:35])[CH:30]=3)=[CH:24][C:23]=2[F:36])=[O:20])[N:8]([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][OH:17])=[CH:12][CH:11]=2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2].C([O-])([O-])=O.[K+].[K+].CS(Cl)(=O)=O.[CH3:48][O:49][CH2:50][CH2:51]O.C([O-])([O-])=O.[Na+].[Na+]>C1COCC1.CCOC(C)=O>[C:1]([C:5]1[CH:6]=[C:7]([NH:18][C:19]([NH:21][C:22]2[CH:27]=[CH:26][C:25]([O:28][C:29]3[CH:34]=[CH:33][N:32]=[C:31]([CH3:35])[CH:30]=3)=[CH:24][C:23]=2[F:36])=[O:20])[N:8]([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][O:17][CH2:51][CH2:50][O:49][CH3:48])=[CH:12][CH:11]=2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 80192-MethoxyethanolHCID 10340Sodium CarbonateHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 115332541-[5-tert-Butyl-2-(4-hydroxymethyl-phenyl)-2H-pyrazol-3-yl]-3-[2-fluoro-4-(2-methyl-Pyridin-4-yloxy)-phenyl)-urea

生成物 1

HCID 11649659
1-{5-tert-Butyl-2-[4-(2-methoxy-ethoxymethyl)-phenyl]-2H-pyrazol-3-yl}-3-[2-fluoro-4-(2-methyl-pyridin-4-yloxy)-phenyl]-urea

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-[5-tert-butyl-2-(4-hydroxymethyl-phenyl)-2H-pyrazol-3-yl]-3-[2-fluoro-4-(2-methyl-pyridin-4-yloxy)-phenyl)-urea (170 mg, 0.35 mmol) in anhydrous THF was added K2CO3 (52 mg, 0.38 mmol) followed by methanesulfonyl chloride (30 μL, 0.38 mmol). The mixture was stirred at room temperature for one day, and then 2-methoxy-ethanol (213 mg, 3.5 mmol) was added. The mixture was stirred at room temperature overnight, then EtOAc was added followed by saturated Na2CO3. The organic layer was washed with saturated Na2CO3 and brine, dried over MgSO4 and evaporated at reduced pressure. Purification by HPLC (10% to 90% aq acetonitrile afforded pure product (10 mg, 5%). 1H-NMR (CD3OD) δ 8.17 (d, J=6.0 Hz, 1H), 8.01 (t, J=9.3 Hz, 1H), 7.48-7.37 (m, 4H), 6.93-6.69 (m, 4H), 6.36 (s, 1H), 4.54 (s, 2H), 3.58 (m, 2H), 3.50 (m, 2H), 3.28 (s, 3H), 2.37 (s, 3H), 1.25 (s, 9H); MS LC-MS [M+H]+=548.1, RT=2.69 min.

後処理

  1. stirringThe mixture was stirred at room temperature overnight
  2. washThe organic layer was washed with saturated Na2CO3 and brine
  3. dry with materialdried over MgSO4
  4. customevaporated at reduced pressure
  5. customPurification by HPLC (10% to 90% aq acetonitrile afforded pure product (10 mg, 5%)

出典と根拠

ORDレコード
ord-f069ed2db08643889d45a55f1d2429ef
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08207166B2

反応ノート

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