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Tris(furan-2-yl)phosphane → HCID 2819962, 화합물

HRID 564224
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HRID 564224 반응식
Br[C:2]1[S:6][C:5]([C:7]([O:9][CH3:10])=[O:8])=[CH:4][CH:3]=1.O1C=CC=C1P(C1OC=CC=1)C1OC=CC=1.C([Sn](CCCC)(CCCC)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=1)CCC>CN(C=O)C>[N:33]1[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=1[C:2]1[S:6][C:5]([C:7]([O:9][CH3:10])=[O:8])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 521585Tris(furan-2-yl)phosphaneHCID 605713Methyl 5-bromothiophene-2-carboxylateHCID 6077842-(Tributylstannyl)pyridine

생성물 1

HCID 2819962HCID 2819962, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

To methyl 5-bromo-thiophene-2-carboxylate (2 g), tri-2-furylphosphine (400 mg), and tris(dibenzylidineacetone)dipalladium(0) (400 mg) was added DMF (50 mL), 2-(tributylstannyl)pyridine (4 g) and TEA (1 mL) The mixture was heated at 80° C. for 7 hours, cooled and partitioned between ethyl acetate and brine. The aqueous phase was extracted with ethyl acetate, and the extract was dried, filtered and concentrated. The concentrate was flash chromatographed on silica gel with a 20-70% ethyl acetate in hexane.

후처리

  1. temperaturecooled
  2. custompartitioned between ethyl acetate and brine
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. customthe extract was dried
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customchromatographed on silica gel with a 20-70% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-6bb7061b7e5f463fbdbdbfab265cbcbf
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08067613B2

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