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Sodium Hydroxide → HCID 22329188, 화합물

HRID 587085
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HRID 587085 반응식
[CH2:1]([O:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][C:18]3[N:24]([CH2:25][CH2:26][CH2:27][O:28][CH3:29])[CH2:23][CH2:22][C:21]([C:30]([O:32]C)=[O:31])=[CH:20][C:19]=3[CH:34]=2)=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH3:4].[OH-].[Na+]>C1COCC1.CO>[CH2:1]([O:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][C:18]3[N:24]([CH2:25][CH2:26][CH2:27][O:28][CH3:29])[CH2:23][CH2:22][C:21]([C:30]([OH:32])=[O:31])=[CH:20][C:19]=3[CH:34]=2)=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH3:4]
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4

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HCID 14798Sodium HydroxideHCID 22329170methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(3-methoxypropyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate

생성물 1

HCID 22329188HCID 22329188, 화합물수율 80.5%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

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온도
50 °C

실험 절차

To a solution of methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(3-methoxypropyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate (362.3 mg) in a mixture of THF-methanol (5-10 ml) was added 1N sodium hydroxide solution (2.8 ml) at room temperature, and the mixture was stirred at 50° C. for 15 hours. After concentration under reduced pressure, 1N hydrochloric acid was added to pH 3-4, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried with magnesium sulfate. After concentration under reduced pressure, the resulting crystals were collected by filtration. The crystals were washed with diisopropyl ether and hexane to give 7-[4-(2-butoxyethoxy)phenyl]-1-(3-methoxypropyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid (283 mg) as yellow crystals.

후처리

  1. concentrationAfter concentration under reduced pressure, 1N hydrochloric acid
  2. additionwas added to pH 3-4
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried with magnesium sulfate
  6. concentrationAfter concentration under reduced pressure
  7. filtrationthe resulting crystals were collected by filtration
  8. washThe crystals were washed with diisopropyl ether and hexane

출처 및 근거

ORD 기록
ord-903907b2d7bf430d981fef412ad1e047
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06936602B1

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