Hydrochloric Acid → 1-formyl-7-[4-(2-propoxy)ethoxyphenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid

HRID 586877노트

반응식

HRID 586877 반응식
[CH:1]([N:3]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][O:23][CH:24]([CH3:26])[CH3:25])=[CH:16][CH:15]=3)=[CH:13][C:8]=2[CH:7]=[C:6]([C:27]([O:29]C)=[O:28])[CH2:5][CH2:4]1)=[O:2].[OH-].[Na+].Cl>C1COCC1.C(O)C>[CH:1]([N:3]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][O:23][CH:24]([CH3:25])[CH3:26])=[CH:16][CH:15]=3)=[CH:13][C:8]=2[CH:7]=[C:6]([C:27]([OH:29])=[O:28])[CH2:5][CH2:4]1)=[O:2]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22329024methyl 1-formyl-7-[4-(2-propoxy)ethoxyphenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate

생성물 1

HCID 223293211-formyl-7-[4-(2-propoxy)ethoxyphenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid수율 100.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

In a mixture of THF and ethanol (1:1, v/v, 30.0 ml) was dissolved methyl 1-formyl-7-[4-(2-propoxy)ethoxyphenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (445 mg). To the solution was added 1N sodium hydroxide solution (11.0 ml), and the mixture was stirred at room temperature for 13 hours. The mixture was a little concentrated, and to the residue was added 1N hydrochloric acid to convert weakly acidic solution. The mixture was extracted with ethyl acetate, and the organic layer was washed with water and saturated brine, and dried with anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give crystals, which were washed with ethyl acetate/hexane to give 1-formyl-7-[4-(2-propoxy)ethoxyphenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid (430 mg) as white crystals.

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. washthe organic layer was washed with water and saturated brine
  3. dry with materialdried with anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customto give crystals, which
  6. washwere washed with ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-f98cbbe4e86b4be2a210fa393f4ecac2
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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