홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Cesium carbonate → 2,3,5,6-Tetrafluoro-4'-formyl-biphenyl-4-carboxylic acid methyl ester

HRID 1470661
노트
인쇄 미리보기

반응식

HRID 1470661 반응식
C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:7][O:8][C:9](=[O:21])[C:10]1[C:15]([F:16])=[C:14]([F:17])[C:13](Br)=[C:12]([F:19])[C:11]=1[F:20].B(O)(O)[C:23]1[CH:28]=[CH:27][C:26]([CH:29]=[O:30])=[CH:25][CH:24]=1>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:7][O:8][C:9]([C:10]1[C:15]([F:16])=[C:14]([F:17])[C:13]([C:23]2[CH:28]=[CH:27][C:26]([CH:29]=[O:30])=[CH:25][CH:24]=2)=[C:12]([F:19])[C:11]=1[F:20])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 5910734-Formylphenylboronic AcidHCID 46311226Methyl 4-bromo-2,3,5,6-tetrafluorobenzoate

생성물 1

HCID 580739392,3,5,6-Tetrafluoro-4'-formyl-biphenyl-4-carboxylic acid methyl ester수율 55.24%

시약·촉매·용매 1

HCID 178418476HCID 178418476, 화합물촉매

실험 절차

A toluene/Water (175 mL+25 mL) mixture was degassed with nitrogen for 30 minutes. Cesium carbonate (14.9 g, 43.55 mmol) was added followed by 4-bromo-2,3,5,6-tetrafluoro-benzoic acid methyl ester (5.0 g, 17.42 mmol), 4-formyl boronic acid (3.4 g, 22.64 mmol) and dichlorobis(triphenylphosphine)-palladium(II) catalyst (0.611 g, 0.87 mmol). The reaction mixture was refluxed for 15 h. TLC shows completion of the reaction. The reaction mixture was cooled to room temperature and was extracted with ethyl acetate. The combined organic layers were dried over sodium sulphate and concentrated. The obtained residue was purified by column chromatography using 5% ethyl acetate in hexane to get colorless solid (3.0 g, 55.24%).

후처리

  1. customA toluene/Water (175 mL+25 mL) mixture was degassed with nitrogen for 30 minutes
  2. temperatureThe reaction mixture was refluxed for 15 h
  3. customcompletion of the reaction
  4. extractionwas extracted with ethyl acetate
  5. dry with materialThe combined organic layers were dried over sodium sulphate
  6. concentrationconcentrated
  7. customThe obtained residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-c128b4fd1700418fba75ea49be6e0733
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006454B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트