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Sodium Bicarbonate → Ethyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate

HRID 566147
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반응식

HRID 566147 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11](C=O)[CH2:10][CH2:9][C:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:7][C:6]=2[CH:19]=1.C(=O)([O-])O.[Na+]>Cl.C(O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH2:10][CH2:9][C:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:7][C:6]=2[CH:19]=1
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참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 18472216Ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate

생성물 1

HCID 18472278Ethyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate수율 59%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

In 1N hydrochloric acid (25 ml) and ethanol (20 ml) was dissolved ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate (1165 mg), and the mixture was refluxed for 2 hours. The mixture was neutralized with saturated sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate (300 ml). The organic layer was washed with water (100 ml) and dried with anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified with silica gel column chromatography (150 g, hexane/ethyl acetate=9:1) to give ethyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate (628 mg, 59%).

후처리

  1. temperaturethe mixture was refluxed for 2 hours
  2. extractionthe mixture was extracted with ethyl acetate (300 ml)
  3. washThe organic layer was washed with water (100 ml)
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified with silica gel column chromatography (150 g, hexane/ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-1378268b9ece48dbb8488f62d0b2e0f1
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06172061B2

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