Water → 2-(Benzyloxy)-5-iodobenzaldehyde

HRID 269593ノート

反応式

HRID 269593 の反応式
C(=O)([O-])[O-].[K+].[K+].[OH:7][C:8]1[CH:15]=[CH:14][C:13]([I:16])=[CH:12][C:9]=1[CH:10]=[O:11].[CH2:17](Cl)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O>CN(C)C=O>[CH2:17]([O:7][C:8]1[CH:15]=[CH:14][C:13]([I:16])=[CH:12][C:9]=1[CH:10]=[O:11])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

6

反応物 4

HCID 962WaterHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 2526125-Iodosalicylaldehyde

生成物 1

HCID 150434892-(Benzyloxy)-5-iodobenzaldehyde

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

67.2 g (0.48 mol) of potassium carbonate are added to a solution of 100 g (0.40 mol) of 2-hydroxy-5-iodobenzaldehyde (Example 1A) in 1.5 l of dimethylformamide and, after a few minutes, 51 ml (0.44 mol) of benzyl chloride are added. The reaction mixture is stirred under reflux at 120° C. for 24 h. After stirring at RT for a further 24 h and the addition of 1.5 l of water, a solid crystallizes out. The precipitate is collected by suction filtration, washed twice with water and dried in vacuo. The solid is recrystallized from 230 ml of ethanol. 122.9 g (90% of theory) of product are obtained.

後処理

  1. stirringAfter stirring at RT for a further 24 h
  2. customa solid crystallizes out
  3. filtrationThe precipitate is collected by suction filtration
  4. washwashed twice with water
  5. customdried in vacuo
  6. customThe solid is recrystallized from 230 ml of ethanol
  7. custom122.9 g (90% of theory) of product are obtained

出典と根拠

ORDレコード
ord-9e94ef8973c342148286ee8d143e61ba
出典データセット
uspto-grants-2008_11
特許番号
US07446102B2

反応ノート

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