Sodium Iodide → HCID 18938755、化合物

HRID 356579ノート

反応式

HRID 356579 の反応式
[CH3:1][O:2][CH:3]([O:14][CH3:15])[C:4]1[CH:9]=[C:8]([OH:10])[CH:7]=[CH:6][C:5]=1[N+:11]([O-:13])=[O:12].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Cl[CH2:25][CH2:26][CH2:27][OH:28]>CN(C=O)C.C(OCC)(=O)C>[CH3:15][O:14][CH:3]([O:2][CH3:1])[C:4]1[CH:9]=[C:8]([O:10][CH2:25][CH2:26][CH2:27][OH:28])[CH:7]=[CH:6][C:5]=1[N+:11]([O-:13])=[O:12]

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 123133-Chloro-1-propanolHCID 32847943-(Dimethoxymethyl)-4-nitrophenol

生成物 1

HCID 18938755HCID 18938755、化合物収率 94.2%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

5-Hydroxy-2-nitrobenzaldehyde dimethyl acetal (5.33 g) is dissolved in dry DMF (50 ml), and thereto are added potassium carbonate (6.91 g), sodium iodide (7.5 g) and 3-chloropropanol (4.73 g), and the mixture is stirred at 70° C. for 22 hours. To the mixture is added ethyl acetate, and the insoluble materials are removed by filtration. The filtrate is concentrated under reduced pressure, and the residue is purified by silica gel column chromatography to give 5-(3'-hydroxypropyloxy)-2-nitrobenzaldehyde dimethyl acetal (6.39 g) as a pale yellow oil.

後処理

  1. customthe insoluble materials are removed by filtration
  2. concentrationThe filtrate is concentrated under reduced pressure
  3. customthe residue is purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-bb242bafddaf46b0b4bcd1556637bb8a
出典データセット
uspto-grants-1998_11
特許番号
US05837673

反応ノート

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