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Water → 2-(4-Fluorophenyl)-3-(pyridin-4-yl)-4-(2,4,6-trifluorobenzoylaminomethyl)-1H-pyrrole

HRID 1244986
ノート
印刷プレビュー

反応式

HRID 1244986 の反応式
C(N(CC)CC)C.[F:8][C:9]1[CH:17]=[C:16]([F:18])[CH:15]=[C:14]([F:19])[C:10]=1[C:11](Cl)=[O:12].Cl.Cl.[NH2:22][CH2:23][C:24]1[C:25]([C:36]2[CH:41]=[CH:40][N:39]=[CH:38][CH:37]=2)=[C:26]([C:29]2[CH:34]=[CH:33][C:32]([F:35])=[CH:31][CH:30]=2)[NH:27][CH:28]=1.O>O1CCCC1>[F:35][C:32]1[CH:31]=[CH:30][C:29]([C:26]2[NH:27][CH:28]=[C:24]([CH2:23][NH:22][C:11](=[O:12])[C:10]3[C:9]([F:8])=[CH:17][C:16]([F:18])=[CH:15][C:14]=3[F:19])[C:25]=2[C:36]2[CH:41]=[CH:40][N:39]=[CH:38][CH:37]=2)=[CH:34][CH:33]=1
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 8471TriethylamineHCID 1448952,4,6-Trifluorobenzoyl chlorideHCID 219227564-Aminomethyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole Dihydrochloride

生成物 1

HCID 219228152-(4-Fluorophenyl)-3-(pyridin-4-yl)-4-(2,4,6-trifluorobenzoylaminomethyl)-1H-pyrrole収率 38.5%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

265 μl (1.905 mmol) of triethylamine and 96 mg (0.493 mmol) of 2,4,6-trifluorobenzoyl chloride were added to a suspension of 162 mg (0.476 mmol) of 4-aminomethyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole dihydrochloride [prepared as described in Example 5 above] in 3.3 ml of tetrahydrofuran. The resulting mixture was stirred at room temperature for 4 hours. At the end of this time, water was added to the reaction mixture and then this was extracted with ethyl acetate. The organic extract was washed with water, dried over anhydrous sodium sulfate and then concentrated by evaporation under reduced pressure. The residue thus obtained was washed with diethylether to give 78 mg (yield 38%) of the title compound as a pale yellow powder.

後処理

  1. extractionthis was extracted with ethyl acetate
  2. extractionThe organic extract
  3. washwas washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated by evaporation under reduced pressure
  6. customThe residue thus obtained
  7. washwas washed with diethylether

出典と根拠

ORDレコード
ord-3c9ae1676760426786d0f50d0fce1738
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07122666B2

反応ノート

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