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Benzaldehyde → 2,4-Di(prop-1-en-2-yl)dibenzo[b,d]thiophen-3-amine

HRID 1750926
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HRID 1750926 반응식
Br[C:2]1[C:14]([NH2:15])=[C:13](Br)[C:5]2[S:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:4]=2[CH:3]=1.[CH3:17][C:18]1(C)[C:22](C)(C)OB(C(C)=C)O1.[CH:29](=O)[C:30]1C=CC=C[CH:31]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>C(OCC)(=O)C.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].O.C1(C)C=CC=CC=1>[CH2:17]=[C:18]([C:2]1[C:14]([NH2:15])=[C:13]([C:30]([CH3:31])=[CH2:29])[C:5]2[S:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:4]=2[CH:3]=1)[CH3:22]
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참가 물질

9

반응물 4

HCID 240BenzaldehydeHCID 62657Potassium Phosphate, TribasicHCID 109974264,4,5,5-Tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolaneHCID 584010402,4-Dibromodibenzo[b,d]thiophen-3-amine

생성물 1

HCID 584009962,4-Di(prop-1-en-2-yl)dibenzo[b,d]thiophen-3-amine수율 95%

시약·촉매·용매 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 962Water용매
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

실험 절차

To a degassed toluene (200 mL), 2,4-dibromodibenzo[b,d]thiophen-3-amine (12.15 g, 34.0 mmol), 4,4,5,5-tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolane (17.15 g, 102 mmol), benzaldehyde (3.61 g, 34.0 mmol), potassium phosphate (23.51 g, 102 mmol) dicyclohexyl(2′,6′-dimethoxy-[1,1′-biphenyl]-2-yl)phosphine (1.676 g, 4.08 mmol) and Pd2(dba)3 (0.935 g, 1.021 mmol) and water (20 mL) were sequentially added. The solution was refluxed for overnight in an atmosphere of nitrogen and then allowed to cool to room temperature. The reaction was diluted with ethyl acetate and the organic phase was separated from the aqueous phase. The organic phase was dried over sodium sulfate and the solvent was removed under vacuum. The product was chromatographed using silica gel with ethylacetate and hexanes as the eluent. The solvent was removed to give the title compound (9.0, 95%).

후처리

  1. temperatureThe solution was refluxed for overnight in an atmosphere of nitrogen
  2. customthe organic phase was separated from the aqueous phase
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customthe solvent was removed under vacuum
  5. customThe product was chromatographed
  6. customThe solvent was removed

출처 및 근거

ORD 기록
ord-03171f66983c42f68f9f6cbdfa382131
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156870B2

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