Ammonia → HCID 178522272、化合物

HRID 34030

反応式

HRID 34030 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:26][C:27]([C:29]2[O:30][CH:31]=[CH:32][CH:33]=2)=[O:28])[CH:5]=[C:6]2[C:10]=1[N:9](C(C1OC=CC=1)=O)[N:8]=[C:7]2/[CH:18]=[CH:19]/[C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1.N>C(O)C.[Cl-].[Na+].O>[F:1][C:2]1[CH:3]=[C:4]([NH:26][C:27]([C:29]2[O:30][CH:31]=[CH:32][CH:33]=2)=[O:28])[CH:5]=[C:6]2[C:10]=1[NH:9][N:8]=[C:7]2[CH:18]=[CH:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1

参加物

5

反応物 2

HCID 222AmmoniaHCID 59797182Furan-2-carboxylic acid {7-fluoro-1-(furan-2-carbonyl)-3-[(E)-2-(pyridin-3-yl)-vinyl]-1H-indazole-5-yl}-amide

生成物 1

HCID 178522272HCID 178522272、化合物収率 58.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

208 mg of furan-2-carboxylic acid{7-fluoro-1-(furan-2-carbonyl)-3-[(E)-2-(pyridin-3-yl)-vinyl]-1H-indazol-5-yl}-amide was suspended in 20 mL ethanol, added with 5 mL of concentrated aqueous ammonia and stirred at room temperature overnight. The reaction solution was added with saturated brine, extracted with ethyl acetate, and the organic phase was washed with saturated brine, and dried over magnesium sulfate. The solvent was evaporated, purified by LC-MS and the obtained crystals were suspended in ethyl acetate, neutralized with saturated aqueous sodium hydrogen carbonate, and the organic phase was washed with water and saturated brine, and dried over magnesium sulfate. The solvent was evaporated, to afford 96.2 mg of the title compound as yellow crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. washthe organic phase was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated
  5. custompurified by LC-MS
  6. washthe organic phase was washed with water and saturated brine
  7. dry with materialdried over magnesium sulfate
  8. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-e573073fc06345ba9a52f5d3cadd9a76
出典データセット
uspto-grants-2008_09
特許番号
US07429609B2

関連ノート

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