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Triphenylarsine → HCID 15407933, 화합물

HRID 582042
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HRID 582042 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:44]=[CH:43][C:42]([Cl:45])=[CH:41][N:40]=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:42]1[CH:43]=[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)=[N:40][CH:41]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11773TriphenylarsineHCID 10663122HCID 10663122, 화합물HCID 219426435-Chloro-2-(trimethylstannyl)pyridine

생성물 1

HCID 15407933HCID 15407933, 화합물수율 18.7%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 8857
Ethyl Acetate
용매
HCID 13387N-methyl-2-pyrrolidone용매2회

반응 조건

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 (0.036 g, 0.04 mmol), and AsPh3 (0.098 g, 0.32 mmol) in NMP (5 mL) was added a degassed NMP solution (8 mL) of 2-trimethylstannanyl-5-chloropyridine (~4.0 mmol). The resulting mixture was heated to 60° C. for 16 h, then to 100° C. for a further 2 h. The mixture was then cooled to r.t., diluted with EtOAc, washed 2 times with 10% NH4OH and brine, dried over MgSO4, and concentrated to dryness. The residue was purified by flash chromatography (70% EtOAc/hexanes) followed by a CH2Cl2 /Et2O swish to provide 130 mg of the title compound.

후처리

  1. temperatureThe mixture was then cooled to r.t.
  2. washwashed 2 times with 10% NH4OH and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to dryness
  5. customThe residue was purified by flash chromatography (70% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-d7e1f86846584d53aca07660624c3617
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05922742

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