Hydrochloric Acid → 1-Allyl-7-(4-propoxyethoxyphenyl)-2,3-dihydro-1-benzazepine-4-carboxylic acid

HRID 586981ノート

反応式

HRID 586981 の反応式
[CH2:1]([N:4]1[C:10]2[CH:11]=[CH:12][C:13]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][O:24][CH2:25][CH2:26][CH3:27])=[CH:17][CH:16]=3)=[CH:14][C:9]=2[CH:8]=[C:7]([C:28]([O:30]C)=[O:29])[CH2:6][CH2:5]1)[CH:2]=[CH2:3].[OH-].[Na+].O.Cl>O1CCCC1.CO>[CH2:1]([N:4]1[C:10]2[CH:11]=[CH:12][C:13]([C:15]3[CH:16]=[CH:17][C:18]([O:21][CH2:22][CH2:23][O:24][CH2:25][CH2:26][CH3:27])=[CH:19][CH:20]=3)=[CH:14][C:9]=2[CH:8]=[C:7]([C:28]([OH:30])=[O:29])[CH2:6][CH2:5]1)[CH:2]=[CH2:3]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 69747248Methyl 1-allyl-7-(4-propoxyethoxyphenyl)-2,3-dihydro-1-benzazepine-4-carboxylate

生成物 1

HCID 697493651-Allyl-7-(4-propoxyethoxyphenyl)-2,3-dihydro-1-benzazepine-4-carboxylic acid収率 78.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl 1-allyl-7-(4-propoxyethoxyphenyl)-2,3-dihydro-1-benzazepine-4-carboxylate (262 mg) in a mixture of tetrahydrofuran (19 ml) and methanol (19 ml) was added 1N sodium hydroxide solution (6.3 ml), and the mixture was stirred at room temperature overnight. Then, water and 1N hydrochloric acid were added to make acidic (pH=4) at 0° C., and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with magnesium sulfate. The solvent was evaporated under reduced pressure to give the solid, which was washed with hexane to give 1-allyl-7-(4-propoxyethoxyphenyl)-2,3-dihydro-1-benzazepine-4-carboxylic acid (199 mg) as yellow crystals.

後処理

  1. customat 0° C.
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried with magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customto give the solid, which
  7. washwas washed with hexane

出典と根拠

ORDレコード
ord-e24e4003745447709311af69bede31a5
出典データセット
uspto-grants-2005_08
特許番号
US06936602B1

反応ノート

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