Sodium Hydroxide → HCID 22328990, 화합물

HRID 587087

반응식

HRID 587087 반응식
[CH2:1]([O:3][CH2:4][CH2:5][CH2:6][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][CH3:30])=[CH:20][CH:19]=3)=[CH:17][C:12]=2[CH:11]=[C:10]([C:31]([O:33]C)=[O:32])[CH2:9][CH2:8]1)[CH3:2].[OH-].[Na+]>C1COCC1.CO>[CH2:1]([O:3][CH2:4][CH2:5][CH2:6][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][CH3:30])=[CH:22][CH:23]=3)=[CH:17][C:12]=2[CH:11]=[C:10]([C:31]([OH:33])=[O:32])[CH2:9][CH2:8]1)[CH3:2]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22329178methyl 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate

생성물 1

HCID 22328990HCID 22328990, 화합물수율 84.6%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

To a solution of methyl 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (475 mg) in a mixture of THF-methanol (5-10 ml) was added 1N sodium hydroxide solution (3.0 ml) at room temperature, and the mixture was stirred at 50° C. for 62 hours. After concentration under reduced pressure, to the mixture was added 1N hydrochloric acid (3.0 ml), 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 1-(3-ethoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid (390 mg) as yellow crystals.

후처리

  1. concentrationAfter concentration under reduced pressure
  2. additionto the mixture was added 1N hydrochloric acid (3.0 ml)
  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-4de7716c668b46c7ba13a136eb311e8c
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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