Potassium Carbonate → HCID 22329033, 화합물

HRID 587092노트

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HRID 587092 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][CH2:13][CH3:14])[CH2:10][CH2:9][CH2:8][C:7](=[O:15])[C:6]=2[CH:16]=1.B([O-])([O-])O[C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][O:28][CH2:29][CH2:30][CH2:31][CH3:32])=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C(CCO)=CC=CC=1.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:29]([O:28][CH2:27][CH2:26][O:25][C:22]1[CH:21]=[CH:20][C:19]([C:2]2[CH:3]=[CH:4][C:5]3[N:11]([CH2:12][CH2:13][CH3:14])[CH2:10][CH2:9][CH2:8][C:7](=[O:15])[C:6]=3[CH:16]=2)=[CH:24][CH:23]=1)[CH2:30][CH2:31][CH3:32]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 22329115HCID 22329115, 화합물HCID 867568154-Butoxyethoxyphenyl borate

생성물 1

HCID 22329033HCID 22329033, 화합물수율 86.6%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 66602552Toluene-ethanol water용매

실험 절차

A mixture of 7-bromo-1-propyl-2,3,4,5-tetrahydro-1H-1-benzazepine-5-one (5.89 g), 4-(2-butoxyethoxy)phenyl borate (5.45 g) and potassium carbonate (5.74 g) in toluene-ethanol-water (200-20-20 ml) was stirred at room temperature for 1 hour under argon atmosphere. To the reaction system was added tetrakistriphenylphosphinepalladium (0.72 g), and the mixture was heated to reflux for 3 hours. After cooled to room temperature, 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 residue was separated and purified with column chromatography (ethyl acetate:hexane=1:9→1:4) to give 7-[4-(2-butoxyethoxy)phenyl]-1-propyl-2,3,4,5-tetrahydro-1H-1-benzazepine-5-one (7.15 g) as yellow oil.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 3 hours
  3. temperatureAfter cooled to room temperature
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried with magnesium sulfate
  7. concentrationAfter concentration under reduced pressure
  8. customthe residue was separated
  9. custompurified with column chromatography (ethyl acetate:hexane=1:9→1:4)

출처 및 근거

ORD 기록
ord-462c4ba1925648e084f208cc273c54ad
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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