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

HRID 1801285
ノート
印刷プレビュー

反応式

HRID 1801285 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 the 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
  5. dry with materialthe combined organic layers were 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-1f2ae1c9a0d443a3b3ed7f64cf9c4c43
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08344137B2

反応ノート

読み込み中…

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