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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Tributylvinyltin → HCID 58955123, 화합물

HRID 1990970
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HRID 1990970 반응식
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][CH:6]=[C:5]2[S:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)(=[O:13])=[O:12].[CH2:20]([Sn](CCCC)(CCCC)C=C)[CH2:21]CC>C1(C)C=CC=CC=1.C(OCC)(=O)C.[F-].[K+].CC1C=CC=CC=1[P](C1C=CC=CC=1C)([Pd](Cl)(Cl)[P](C1=C(C)C=CC=C1)(C1C=CC=CC=1C)C1C=CC=CC=1C)C1C=CC=CC=1C>[C:14]1([S:11]([C:5]2[C:4]3[C:8](=[CH:9][CH:10]=[C:2]([CH:20]=[CH2:21])[CH:3]=3)[NH:7][CH:6]=2)(=[O:13])=[O:12])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 81998TributylvinyltinHCID 58955093HCID 58955093, 화합물

생성물 1

HCID 58955123HCID 58955123, 화합물수율 74%

시약·촉매·용매 4

HCID 178424406HCID 178424406, 화합물촉매HCID 1140Toluene용매HCID 8857Ethyl Acetate
용매
HCID 522689Potassium Fluoride용매

실험 절차

5-bromo-3-(phenylsulfonyl)-1H-indole (505 mg, 1.50 mmol) and dichlorobis(tri-o-tolylphosphine)-palladium(II) (118 mg, 0.09 mmol) were dissolved in toluene (5 mL) and stirred for 10 minutes at room temperature under a nitrogen atmosphere. Tributyl(vinyl)tin (619 mg, 1.95 mmol) was added and the mixture was refluxed for 1 hour. The mixture was cooled to room temperature, diluted with ethyl acetate (10 mL), 1 M KF (5 mL) and stirred for 12 hours. The resultant tin salt precipitate is removed by suction filtration and the organic layer was washed with water (5 mL), then brine and dried over MgSO4, filtered and concentrated in vacuo. Purification by flash chromatography (40% ethyl acetate/petroleum ether) gave the title compound as a white solid (313 mg, 74%). Mp: 140-145° C. MS (ES+): 284 (M+H).

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperatureThe mixture was cooled to room temperature
  3. stirringstirred for 12 hours
  4. customThe resultant tin salt precipitate is removed by suction filtration
  5. washthe organic layer was washed with water (5 mL)
  6. dry with materialbrine and dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customPurification by flash chromatography (40% ethyl acetate/petroleum ether)

출처 및 근거

ORD 기록
ord-500896f78b7d432ca14d45e2f83f95a0
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645752B2

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