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Ammonia → 5-(3H-Imidazo[4,5-c]pyridin-3-yl)-3-{1-[2-(trifluoromethyl)phenyl]ethoxy}thiophene-2-carboxamide

HRID 2391581
ノート
印刷プレビュー

反応式

HRID 2391581 の反応式
[N:1]1[C:9]2[CH:8]=[CH:7][N:6]=[CH:5][C:4]=2[N:3]([C:10]2[S:14][C:13]([C:15]([O:17]C)=O)=[C:12]([O:19][CH:20]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[C:28]([F:31])([F:30])[F:29])[CH3:21])[CH:11]=2)[CH:2]=1.[NH3:32]>CO>[N:1]1[C:9]2[CH:8]=[CH:7][N:6]=[CH:5][C:4]=2[N:3]([C:10]2[S:14][C:13]([C:15]([NH2:32])=[O:17])=[C:12]([O:19][CH:20]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[C:28]([F:29])([F:30])[F:31])[CH3:21])[CH:11]=2)[CH:2]=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

4

反応物 2

HCID 222Ammonia2 回HCID 68771304methyl 5-(3H-imidazo[4,5-c]pyridin-3-yl)-3-{1-[2-(trifluoromethyl)phenyl]ethoxy}thiophene-2-carboxylate

生成物 1

HCID 251530805-(3H-Imidazo[4,5-c]pyridin-3-yl)-3-{1-[2-(trifluoromethyl)phenyl]ethoxy}thiophene-2-carboxamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
125 °C

実験手順

A mixture of 92 mg of the above-synthesized methyl 5-(3H-imidazo[4,5-c]pyridin-3-yl)-3-{1-[2-(trifluoromethyl)phenyl]ethoxy}thiophene-2-carboxylate and 10 ml of a saturated solution of ammonia in methanol was stirred in a microwave vial at 125° C. for 4 h in the microwave cavity. The reaction mixture was allowed to come to room temperature, then another 10 ml of a saturated solution of ammonia in methanol were added and the procedure was repeated as described above. The solvent was removed under vacuum and the residue was purified by flash chromatography (n-hexane/ethyl acetate, elution gradient 10/0 to 3/7 (v/v)) to give the title compound.

後処理

  1. customto come to room temperature
  2. customThe solvent was removed under vacuum
  3. customthe residue was purified by flash chromatography (n-hexane/ethyl acetate, elution gradient 10/0 to 3/7 (v/v))

出典と根拠

ORDレコード
ord-816bdfe7c2db4622886d713e28af4354
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273890B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート