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Water → Methyl 7-bromo-1-(2-thienylcarbonyl)-2,3-dihydro-1-benzazepine-4-carboxylate

HRID 587023
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HRID 587023 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH2:10][CH2:9][C:8]([C:12]([O:14][CH3:15])=[O:13])=[CH:7][C:6]=2[CH:16]=1.N1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[S:23]1C=CC=C1Cl.[OH2:29]>O1CCCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:18]([C:19]3[S:23][CH:22]=[CH:21][CH:20]=3)=[O:29])[CH2:10][CH2:9][C:8]([C:12]([O:14][CH3:15])=[O:13])=[CH:7][C:6]=2[CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 72992-ChlorothiopheneHCID 22328963Methyl 7-bromo-2,3-dihydro-1H-1-benzazepine-4-carboxylate

생성물 1

HCID 22329012Methyl 7-bromo-1-(2-thienylcarbonyl)-2,3-dihydro-1-benzazepine-4-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

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온도
78 °C

실험 절차

To a solution of methyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate (200 mg) and pyridine (123 mg) in tetrahydrofuran (10 ml) was added 2-thienyl chloride (208 mg) at 0° C., and the mixture was heated at 78° C. overnight. After allowing to cool, to the mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with magnesium sulfate. The solvent was evaporated, which was recrystallized from hexane-ethyl acetate to give methyl 7-bromo-1-(2-thienylcarbonyl)-2,3-dihydro-1-benzazepine-4-carboxylate (236 mg) as colorless crystals.

후처리

  1. temperatureto cool, to the mixture
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated brine
  4. dry with materialdried with magnesium sulfate
  5. customThe solvent was evaporated
  6. customwhich was recrystallized from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-1ffd5f06a8b64fbd800d5841614c67fb
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06936602B1

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