Ethanol → 4-Bromo-2-(diethoxymethyl)-1-iodobenzene

HRID 716796ノート

反応式

HRID 716796 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].[CH3:11][C:12]1C=CC(S(O)(=O)=O)=CC=1.[CH2:22]([OH:24])[CH3:23]>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:10])=[C:6]([CH:7]([O:24][CH2:22][CH3:23])[O:8][CH2:11][CH3:12])[CH:9]=1

参加物

4

反応物 3

HCID 702EthanolHCID 6101p-Toluenesulfonic acidHCID 219738615-Bromo-2-iodobenzaldehyde

生成物 1

HCID 672964774-Bromo-2-(diethoxymethyl)-1-iodobenzene

実験手順

A mixture of 5-bromo-2-iodobenzaldehyde (14.9) (1.0 g, 3.2 mmol) and PTSA (0.1 g) in ethanol was stirred under reflux for 18 hrs and concentrated under reduced pressure. The residue was dissolved in ethyl acetate and washed with saturated NaHCO3, dried over anhydrous Na2SO4 and concentrated to give 4-bromo-2-(diethoxymethyl)-1-iodobenzene (14.10) that was directly used in next reaction without further purification.

後処理

  1. temperatureunder reflux for 18 hrs
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with saturated NaHCO3
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-aa015ce35649414c894c6eb59c6b704b
出典データセット
uspto-grants-2015_11
特許番号
US09193669B2

反応ノート

読み込み中…