Diethyl Ether → HCID 67195875, 화합물

HRID 1530172노트

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HRID 1530172 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5](I)=[CH:4][C:3]=1[F:9].CC1(C)C(C)(C)OB([C:18]2[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][OH:27])=[CH:20][CH:19]=2)O1.CCOCC>O.C1COCC1.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>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:18]2[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][OH:27])=[CH:20][CH:19]=2)=[CH:4][C:3]=1[F:9]

참가 물질

7

반응물 3

HCID 3283Diethyl EtherHCID 27250061-Bromo-2-fluoro-4-iodobenzeneHCID 586855993-[4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]propan-1-ol

생성물 1

HCID 67195875HCID 67195875, 화합물

시약·촉매·용매 3

HCID 178418476HCID 178418476, 화합물촉매HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

18 g (65 mmol) of sodium metaborate octahydrate and 2.8 g (3.9 mmol) of bis(triphenylphosphine)palladium(II) chloride are initially introduced in 200 ml of water and 100 ml of THF, 1-bromo-2-fluoro-4-iodobenzene are added, and a solution of 21.5 g (0.082 mol) of 3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]propan-1-ol in 100 ml THF is subsequently added dropwise. The batch is heated under reflux overnight, taken up in MTB ether and washed three times with water. The org. phase is dried over sodium sulfate, and the solvent is removed in vacuo. Chromatography of the crude product on silica gel with toluene/ethyl acetate (7:1) gives 3-(4′-bromo-3′-fluorobiphenyl-4-yl)propan-1-ol as a colourless oil.

후처리

  1. temperatureThe batch is heated
  2. temperatureunder reflux overnight
  3. washwashed three times with water
  4. dry with materialphase is dried over sodium sulfate
  5. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-effd202c224940a2a5451be7e505ed88
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09090822B2

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