Hydrochloric Acid → Methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate

HRID 586833노트

반응식

HRID 586833 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9][C:8]([C:19]([O:21][CH3:22])=[O:20])=[CH:7][C:6]=2[CH:23]=1.Cl.[OH-].[Na+]>C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH2:10][CH2:9][C:8]([C:19]([O:21][CH3:22])=[O:20])=[CH:7][C:6]=2[CH:23]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 22329270HCID 22329270, 화합물

생성물 1

HCID 22328963Methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate수율 90.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

In ethyl acetate (50 ml) was dissolved methyl 7-bromo-1-(t-butoxycarbonyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1.5 g). To the solution was added 6N hydrochloric acid (2 ml), and the mixture was heated to stir at 80° C. for 2 hours, neutralized with 1N sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with anhydrous magnesium sulfate. The solvent was evaporated to give methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1.0 g) as yellow crystals.

후처리

  1. temperaturethe mixture was heated
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-9d37eefaa9f248b6b2a0bcd0c35b94d2
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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