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

HRID 586981노트

반응식

HRID 586981 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e24e4003745447709311af69bede31a5
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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