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Hydrochloric Acid → 7-Bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid

HRID 566144
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반응식

HRID 566144 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH:12]=[O:13])[CH2:10][CH2:9][C:8]([C:14]([O:16]CC)=[O:15])=[CH:7][C:6]=2[CH:19]=1.Cl>[OH-].[Na+].C1COCC1.C(O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH:12]=[O:13])[CH2:10][CH2:9][C:8]([C:14]([OH:16])=[O:15])=[CH:7][C:6]=2[CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 18472216Ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate

생성물 1

HCID 184725177-Bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid수율 100%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide용매HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

In 1N sodium hydroxide (13.0 ml) and THF:ethanol (1:1, 50 ml) was dissolved ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate (2.77 g), and the mixture was stirred at room temperature for 15 hours. To the mixture was added 1N hydrochloric acid (12.5 ml), and the mixture was concentrated. To the residue was added water (200 ml), and the mixture was adjusted to pH 2 with 1N hydrochloric acid. The mixture was extracted with ethyl acetate(300 ml×3), and the organic layer was dried with magnesium sulfate. The solvent was evaporated under reduced pressure to give 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylic acid (2.52 g, 100%).

후처리

  1. concentrationthe mixture was concentrated
  2. additionTo the residue was added water (200 ml)
  3. extractionThe mixture was extracted with ethyl acetate(300 ml×3)
  4. dry with materialthe organic layer was dried with magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-43915a424f4345c4b4584769d254a322
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06172061B2

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