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Water → 6-Fluoro-3-[(E)-2-(3-fluorophenyl)-vinyl]-1-trityl-1H-indazole-5-carboxylic Acid

HRID 34017
ノート
印刷プレビュー

反応式

HRID 34017 の反応式
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6](/[CH:11]=[CH:12]/[C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)=[N:7][NH:8]2)=[CH:4][C:3]=1[C:20]([OH:22])=[O:21].[H-].[Na+].[C:25](Cl)([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.O>CN(C)C=O>[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6](/[CH:11]=[CH:12]/[C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([F:19])[CH:14]=3)=[N:7][N:8]2[C:25]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)([C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=2)[C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)=[CH:4][C:3]=1[C:20]([OH:22])=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6456Trityl chlorideHCID 24758Sodium hydrideHCID 59797186HCID 59797186、化合物

生成物 1

HCID 689303146-Fluoro-3-[(E)-2-(3-fluorophenyl)-vinyl]-1-trityl-1H-indazole-5-carboxylic Acid収率 58.5%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

Under ice cooling, to a solution of 350 mg of 6-fluoro-3-[(E)-2-(3-fluorophenyl)-vinyl]-1H-indazole-5-carboxylic acid obtained by Example 101 in 6 mL of N,N-dimethylformamide was added 103 mg of 60% sodium hydride, stirred for 30 minutes, then added with 390 mg of trityl chloride, and stirred at this temperature for 20 minutes and at room temperature for 1 hour. The reaction solution was added with water and extracted with 80 mL of ethyl acetate. The organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified and separated by silica gel column chromatography (ethylacetate:toluene=1:9), to afford 370 mg of the title compound as bright yellow crystals.

後処理

  1. stirringstirred at this temperature for 20 minutes and at room temperature for 1 hour
  2. extractionextracted with 80 mL of ethyl acetate
  3. washThe organic layer was washed successively with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe crude product was purified
  7. customseparated by silica gel column chromatography (ethylacetate:toluene=1:9)

出典と根拠

ORDレコード
ord-d65698d886434ecb9ac6328f52823d70
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429609B2

反応ノート

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