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Sodium Carbonate → HCID 66777760, 화합물

HRID 2091388
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HRID 2091388 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10](=[O:14])[CH:11]([CH3:13])[CH3:12])=[C:7]([CH3:15])[C:6]=2[CH:16]=1.[CH:17]1(B(O)O)[CH2:19][CH2:18]1.C(=O)([O-])[O-].[Na+].[Na+].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH:17]1([C:2]2[CH:3]=[CH:4][C:5]3[O:9][C:8]([C:10](=[O:14])[CH:11]([CH3:13])[CH3:12])=[C:7]([CH3:15])[C:6]=3[CH:16]=2)[CH2:19][CH2:18]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10340Sodium CarbonateHCID 2760897Cyclopropylboronic acidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 290760271-(5-Bromo-3-methyl-1-benzofuran-2-yl)-2-methylpropan-1-one

생성물 1

HCID 66777760HCID 66777760, 화합물수율 93%

시약·촉매·용매 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 1140Toluene용매

실험 절차

To a solution (20 mL) of 1-(5-bromo-3-methyl-1-benzofuran-2-yl)-2-methylpropan-1-one (1.0 g) synthesized in Example A182(1) in toluene were added cyclopropaneboronic acid (0.92 g), 2N aqueous sodium carbonate solution (5.3 mL), and the mixture was stirred at room temperature for 10 min under argon atmosphere. To the reaction mixture were added 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (0.18 g) and tris(dibenzylideneacetone)dipalladium (0) (0.10 g), and the mixture was heated under reflux under argon atmosphere overnight. The reaction mixture was cooled to room temperature, and filtered through celite, and the residue was washed with diethyl ether. Water was added to the filtrate, and the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:10, volume ratio) to give the title object compound (0.80 g, 93%) as a yellow oil.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux under argon atmosphere overnight
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationfiltered through celite
  5. washthe residue was washed with diethyl ether
  6. additionWater was added to the filtrate
  7. concentrationthe organic layer was concentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:10, volume ratio)

출처 및 근거

ORD 기록
ord-c5775248c8324daf8ba322e73b5aa8bc
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436043B2

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