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Isobutyraldehyde → Methyl 4-hydroxy-3,3-dimethyl-2-(4-nitrophenyl)-1,2,3,4-tetrahydroquinoline-6-carboxylate

HRID 2045564
ノート
印刷プレビュー

反応式

HRID 2045564 の反応式
[N+:1]([C:4]1[CH:21]=[CH:20][C:7](/[CH:8]=[N:9]/[C:10]2[CH:19]=[CH:18][C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][CH:11]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH:22](=[O:26])[CH:23]([CH3:25])[CH3:24]>O1CCCC1.FC(F)(F)S([O-])(=O)=O.[Y+3].FC(F)(F)S([O-])(=O)=O.FC(F)(F)S([O-])(=O)=O>[OH:26][CH:22]1[C:19]2[C:10](=[CH:11][CH:12]=[C:13]([C:14]([O:16][CH3:17])=[O:15])[CH:18]=2)[NH:9][CH:8]([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:21][CH:20]=2)[C:23]1([CH3:25])[CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6561IsobutyraldehydeHCID 178498134HCID 178498134、化合物

生成物 1

HCID 67443026Methyl 4-hydroxy-3,3-dimethyl-2-(4-nitrophenyl)-1,2,3,4-tetrahydroquinoline-6-carboxylate収率 20%

試薬・触媒・溶媒 2

HCID 2733939Yttrium trifluoromethanesulfonate触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (E)-methyl 4-(4-nitrobenzylideneamino)benzoate (284 mg 1 mmol) and yttrium(III) trifluoromethanesulfonate (62 mg, 0.1 mmol) in tetrahydrofuran (5 mL) was added isobutyraldehyde (72 mg, 1.5 mmol). The resultant mixture was stirred at room temperature for 16 h. Thin layer chromatography showed the starting material was completely consumed. The reaction mixture was quenched with water and separated. The aqueous solution was extracted with dichloromethane and he combined organic layers were dried over anhydrous sodium sulfate. Solvent was removed in vacuo to give the crude product, which was purified by column chromatography (petroleum ether/ethyl acetate=3:1) to afford 70 mg of methyl 4-hydroxy-3,3-dimethyl-2-(4-nitrophenyl)-1,2,3,4-tetrahydroquinoline-6-carboxylate as a yellow solid. Yield: 20%.

後処理

  1. customwas completely consumed
  2. customThe reaction mixture was quenched with water
  3. customseparated
  4. extractionThe aqueous solution was extracted with dichloromethane and he
  5. dry with materialwere dried over anhydrous sodium sulfate
  6. customSolvent was removed in vacuo
  7. customto give the crude product, which
  8. customwas purified by column chromatography (petroleum ether/ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-67d38f57154943889ffcc2654943dd1e
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586747B2

反応ノート

読み込み中…

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