Benzyl Bromide → HCID 68431966、化合物

HRID 2267005ノート

反応式

HRID 2267005 の反応式
[CH2:1](Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I:9][C:10]1[C:15]([OH:16])=[CH:14][CH:13]=[CH:12][C:11]=1O.[C:18](=[O:21])([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[CH2:1]([O:16][C:15]1[CH:14]=[CH:13][CH:12]=[C:11]([O:21][CH2:18][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:10]=1[I:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 10796Cesium carbonateHCID 6168332-iodobenzene-1,3-diol

生成物 1

HCID 68431966HCID 68431966、化合物収率 71.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Add benzyl bromide (7.97 g, 46.6 mmol) to a solution of 2-iodo-benzene-1,3-diol (5.00 g, 21.2 mmol) and cesium carbonate (15.2 g, 46.6 mmol) in dimethylformamide (200 mL) and stir. After 18 hours, concentrate under reduced pressure. Add water (500 mL) and stir. After 1 hour, filter the resulting precipitate washing with water and hexanes to yield the title compound as an off-white solid (6.30 g, 71%): 1H NMR (CDCl3) δ 5.18 (s, 4H), 6.55 (d, 2H), 7.19 (t, 1H), 7.29-7.53 (m, 10H).

後処理

  1. concentrationconcentrate under reduced pressure
  2. stirringAdd water (500 mL) and stir
  3. waitAfter 1 hour
  4. filtrationfilter the resulting precipitate
  5. washwashing with water and hexanes

出典と根拠

ORDレコード
ord-0b9c62b785374723a61f3d84a3e797b8
出典データセット
uspto-grants-2010_12
特許番号
US07858646B2

反応ノート

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