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Triphenylarsine → 2-(5-Chloro-pyridin-3-yl)-3-(4-methanesulfonyl-phenyl)-cyclopent-2-enone

HRID 582038
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HRID 582038 반응식
Br[C:2]1[C:3](=[O:17])[CH2:4][CH2:5][C:6]=1[C:7]1[CH:12]=[CH:11][C:10]([S:13]([CH3:16])(=[O:15])=[O:14])=[CH:9][CH:8]=1.C1C=CC([As](C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C[Sn](C)(C)[C:39]1[CH:40]=[N:41][CH:42]=[C:43]([Cl:45])[CH:44]=1>CN1C(=O)CCC1.CCOC(C)=O.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]>[Cl:45][C:43]1[CH:44]=[C:39]([C:2]2[C:3](=[O:17])[CH2:4][CH2:5][C:6]=2[C:7]2[CH:12]=[CH:11][C:10]([S:13]([CH3:16])(=[O:15])=[O:14])=[CH:9][CH:8]=2)[CH:40]=[N:41][CH:42]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11773TriphenylarsineHCID 10663122HCID 10663122, 화합물HCID 675529863-Trimethylstannanyl-5-chloropyridine

생성물 1

HCID 106653622-(5-Chloro-pyridin-3-yl)-3-(4-methanesulfonyl-phenyl)-cyclopent-2-enone수율 30.9%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium
촉매
HCID 8857Ethyl Acetate용매
HCID 13387N-methyl-2-pyrrolidone용매2회

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온도
60 °C

실험 절차

To a degassed r.t. solution of 2-bromo-3-(4-(methylsulfonyl)phenyl)-2-cyclopenten-1-one (0.630 g, 2.0 mmol), Pd2 (dba)3 (0.037 g, 0.04 mmol), and AsPh3 (0.098 g, 0.32 mmol) in 5 mL NMP was added a degassed NMP solution (5 mL) of 3-trimethylstannanyl-5-chloropyridine (~2.0 mmol). The resulting mixture was heated to 60° C. for 16 h. The mixture was then cooled to r.t., diluted with EtOAc, washed with water and brine, dried over MgSO4, and concentrated to dryness. The residue was purified by flash chromatography (80% EtOAc/hexanes) followed by a CH2Cl2 /Et2O swish to provide 0.215 g of the title compound.

후처리

  1. temperatureThe mixture was then cooled to r.t.
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to dryness
  5. customThe residue was purified by flash chromatography (80% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-fbb593b24505420b9b2442cafcd03edc
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05922742

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