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Water → 5-chloro-3-(4,4-difluorocyclohexylmethyl)-N-phenyl-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxamide

HRID 1468287
ノート
印刷プレビュー

反応式

HRID 1468287 の反応式
[Cl:1][C:2]1[N:7]2[C:8]([CH2:15][CH:16]3[CH2:21][CH2:20][C:19]([F:23])([F:22])[CH2:18][CH2:17]3)=[C:9]([C:11]([F:14])([F:13])[F:12])[N:10]=[C:6]2[CH:5]=[C:4]([C:24]([OH:26])=O)[CH:3]=1.CCN=C=NCCCN(C)C.Cl.[CH:39]1[CH:40]=[CH:41][C:42]2N(O)N=[N:45][C:43]=2[CH:44]=1.O.NC1C=CC=CC=1>CN(C=O)C>[Cl:1][C:2]1[N:7]2[C:8]([CH2:15][CH:16]3[CH2:21][CH2:20][C:19]([F:22])([F:23])[CH2:18][CH2:17]3)=[C:9]([C:11]([F:14])([F:12])[F:13])[N:10]=[C:6]2[CH:5]=[C:4]([C:24]([NH:45][C:43]2[CH:44]=[CH:39][CH:40]=[CH:41][CH:42]=2)=[O:26])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 962WaterHCID 6115AnilineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 867100955-Chloro-3-(4,4-difluorocyclohexylmethyl)-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxylic acid

生成物 1

HCID 86710096
5-chloro-3-(4,4-difluorocyclohexylmethyl)-N-phenyl-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxamide
収率 62%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A part of the crude product of 5-chloro-3-(4,4-difluorocyclohexylmethyl)-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxylic acid obtained in step 3 (28 mg) was dissolved in DMF (2.0 mL), and the solution was stirred overnight at room temperature after adding EDC.HCl (27 mg, 0.141 mmol), HOBt.H2O (22 mg, 0.141 mmol), and aniline (13 mg, 0.141 mmol). The reaction mixture was extracted with ethyl acetate after adding a sodium hydrogen carbonate aqueous solution. The organic layer was washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was then evaporated under reduced pressure. The residue was purified by preparative thin-layer chromatography (chloroform/methanol=9/1) to give 5-chloro-3-(4,4-difluorocyclohexylmethyl)-N-phenyl-2-trifluoromethylimidazo[1,2-a]pyridine-7-carboxamide (18.0 mg, two-step yield 62%).

後処理

  1. extractionThe reaction mixture was extracted with ethyl acetate
  2. additionafter adding a sodium hydrogen carbonate aqueous solution
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was then evaporated under reduced pressure
  6. customThe residue was purified by preparative thin-layer chromatography (chloroform/methanol=9/1)

出典と根拠

ORDレコード
ord-039b3402046346d294fd5588e9060bea
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09000186B2

反応ノート

読み込み中…

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