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Methanol → Methyl 3-(3-(diethoxymethyl)phenyl)-4-oxo-2-phenyl-1,2,3,4-tetrahydroquinoline-5-carboxylate

HRID 1467518
ノート
印刷プレビュー

反応式

HRID 1467518 の反応式
[CH:1](=[N:8]/[C:9]1C=CC=[C:14]2[C:10]=1CO[C:13]2=O)\[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:19]([O:21][CH:22]([O:31][CH2:32][CH3:33])[C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[CH:26]=O)[CH3:20].[CH3:34][O-:35].[Na+].CO.[C:39]([O:43][CH2:44]C)(=[O:42])[CH2:40][CH3:41]>>[CH2:19]([O:21][CH:22]([O:31][CH2:32][CH3:33])[C:23]1[CH:24]=[C:25]([CH:26]2[C:34](=[O:35])[C:41]3[C:40]([C:39]([O:43][CH3:44])=[O:42])=[CH:13][CH:14]=[CH:10][C:9]=3[NH:8][CH:1]2[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:28]=[CH:29][CH:30]=1)[CH3:20]
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

6

反応物 5

HCID 887MethanolHCID 7749Ethyl PropionateHCID 10942334Sodium MethoxideHCID 162177103-(Diethoxymethyl)benzaldehydeHCID 178519069HCID 178519069、化合物

生成物 1

HCID 67261363Methyl 3-(3-(diethoxymethyl)phenyl)-4-oxo-2-phenyl-1,2,3,4-tetrahydroquinoline-5-carboxylate収率 25%

反応条件

温度
0 °C

実験手順

A mixture of (E)-4-(benzylideneamino)isobenzofuran-1(3H)-one (474 mg, 2 mmol) and 3-(diethoxymethyl)benzaldehyde (418 mg, 2 mmol) in ethyl propionate (20 mL) was cooled to 0° C. Sodium methoxide in methanol solution [sodium (148 mg, 8 mmol) in methanol (2 mL)] was then added dropwise and the mixture was stirred at room temperature overnight. The resulting mixture was evaporated under reduced pressure. The residue was extracted with ethyl acetate (100 mL×3) and the combined organic layers were washed with brine, dried over anhydrous sodium sulfate and concentrated to give crude product. The crude product was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=50:1 to 5:1) to give methyl 3-(3-(diethoxymethyl)phenyl)-4-oxo-2-phenyl-1,2,3,4-tetrahydroquinoline-5-carboxylate (230 mg, yield 25%) as a yellow solid.

後処理

  1. customThe resulting mixture was evaporated under reduced pressure
  2. extractionThe residue was extracted with ethyl acetate (100 mL×3)
  3. washthe combined organic layers were washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customto give crude product
  7. customThe crude product was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=50:1 to 5:1)

出典と根拠

ORDレコード
ord-4955dbe337eb4e21939c062f2bf60793
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999987B2

反応ノート

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