Hydrochloric Acid → 1-(Allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylic acid

HRID 587063

반응식

HRID 587063 반응식
[CH2:1]([O:4][C:5]([N:7]1[C:13]2[CH:14]=[CH:15][C:16]([C:18]3[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:20][CH:19]=3)=[CH:17][C:12]=2[CH:11]=[C:10]([C:32]([O:34]C)=[O:33])[CH2:9][CH2:8]1)=[O:6])[CH:2]=[CH2:3].[OH-].[Na+].Cl>C1COCC1.C(O)C>[CH2:1]([O:4][C:5]([N:7]1[C:13]2[CH:14]=[CH:15][C:16]([C:18]3[CH:19]=[CH:20][C:21]([O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:22][CH:23]=3)=[CH:17][C:12]=2[CH:11]=[C:10]([C:32]([OH:34])=[O:33])[CH2:9][CH2:8]1)=[O:6])[CH:2]=[CH2:3]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22328895Methyl 1-(allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylate

생성물 1

HCID 223291421-(Allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylic acid수율 85.8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

In THF (4.5 ml)/ethanol (4.5 ml) was dissolved methyl 1-(allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylate (0.30 g). To the solution was added 1N sodium hydroxide (3.0 ml), and the mixture was stirred at room temperature for 4 hours. pH was adjusted to approximate 4 with 1N hydrochloric acid, and the solvent was concentrated to half under reduced pressure. The concentrated material was extracted with ethyl acetate, the extract was washed with saturated brine and dried with magnesium sulfate. The solvent was removed under reduced pressure, and the resulting residue was washed with hexane/ethyl acetate (=8/1) to give 1-(allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylic acid (0.25 g).

후처리

  1. concentrationthe solvent was concentrated to half under reduced pressure
  2. extractionThe concentrated material was extracted with ethyl acetate
  3. washthe extract was washed with saturated brine
  4. dry with materialdried with magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. washthe resulting residue was washed with hexane/ethyl acetate (=8/1)

출처 및 근거

ORD 기록
ord-0cba0a0905f940c385014cbe75d076a0
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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