1-Iodo-4-[(2-methylbut-3-yn-2-yl)oxy]benzene → HCID 10913124, 화합물

HRID 1165195노트

반응식

HRID 1165195 반응식
[CH3:1][C:2]([O:6][C:7]1[CH:12]=[CH:11][C:10]([I:13])=[CH:9][CH:8]=1)([CH3:5])[C:3]#[CH:4]>N1C2C(=CC=CC=2)C=CC=1.CCOCC>[CH3:5][C:2]1([CH3:1])[CH:3]=[CH:4][C:8]2[CH:9]=[C:10]([I:13])[CH:11]=[CH:12][C:7]=2[O:6]1

참가 물질

4

반응물 1

HCID 149335571-Iodo-4-[(2-methylbut-3-yn-2-yl)oxy]benzene

생성물 1

HCID 10913124HCID 10913124, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 7047Quinoline용매

실험 절차

A solution of 1-[(1,1-dimethyl-2-propynyl)oxy]-4-iodobenzene (5.97 g, 20.8 mmol) in quinoline (25 mL) was heated at 170° C. for 2 hours. The reaction was cooled to room temperature and diluted with ether. The reaction mixture was washed with 2N HCl (4X eq. vol.), with brine (2X eq. vol.), dried over anhydrous MgSO4 and concentrated to give crude product. This material was combined with product from an identical reaction and purified by flash chromatography, using 100% petroleum ether elution to give 5.58 g, (79% for the two reactions), of product.

후처리

  1. washThe reaction mixture was washed with 2N HCl (4X eq. vol.), with brine (2X eq. vol.)
  2. dry with materialdried over anhydrous MgSO4
  3. concentrationconcentrated
  4. customto give crude product
  5. customThis material was combined with product from an identical reaction
  6. custompurified by flash chromatography
  7. wash100% petroleum ether elution
  8. customto give 5.58 g

출처 및 근거

ORD 기록
ord-e496ebf3374341c9b30e48e82aa15b71
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04908378

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