1-Iodo-4-[(2-methylbut-3-yn-2-yl)oxy]benzene → HCID 10913124、化合物

HRID 1165195ノート

反応式

HRID 1165195 の反応式
[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

参加物

4

反応物 1

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

生成物 1

HCID 10913124HCID 10913124、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 7047Quinoline溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e496ebf3374341c9b30e48e82aa15b71
出典データセット
uspto-grants-1990_03
特許番号
US04908378

反応ノート

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