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

HRID 1189978ノート

反応式

HRID 1189978 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-7fec32c7e7854cfea01b2c14f6c21bf9
出典データセット
uspto-grants-2014_03
特許番号
US08674137B2

反応ノート

読み込み中…