Dimethylformamide → HCID 18383995、化合物

HRID 2297731ノート

反応式

HRID 2297731 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([OH:11])[C:9]=1[OH:10])[CH:5]=[O:6].[C:12](=[O:15])([O-])[O-].[K+].[K+].[CH3:18][O:19][CH2:20]Cl.[CH3:22]N(C)C=O>>[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([O:11][CH2:22][O:15][CH3:12])[C:9]=1[O:10][CH2:18][O:19][CH3:20])[CH:5]=[O:6]

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 7864Chloromethyl Methyl EtherHCID 11430Potassium CarbonateHCID 836513,4,5-Trihydroxybenzaldehyde

生成物 1

HCID 18383995HCID 18383995、化合物収率 17%

実験手順

3,4,5-Trihydroxybenzaldehyde (628 mg, 3.6 mmol) was dissolved in dimethylformamide (30 mL), and potassium carbonate (2.0 g, 14 mmol) was added thereto, followed by stirring at room temperature for 30 minutes. Next, chloromethyl methyl ether (0.96 mL, 13 mmol) was added thereto, followed by stirring at room temperature for 2 hours. After the conventional post-treatment, the residue was purified by preparative thin layer chromatography (developed with chloroform/methanol=98/2) to give 3-hydroxy-4,5-bis(methoxymethoxy)benzaldehyde (140 mg, yield 17%).

後処理

  1. stirringby stirring at room temperature for 2 hours
  2. customAfter the conventional post-treatment, the residue was purified by preparative thin layer chromatography (developed with chloroform/methanol=98/2)

出典と根拠

ORDレコード
ord-21707e02c84548ddb23ab068bf97fe96
出典データセット
uspto-grants-2002_12
特許番号
US06492392B1

反応ノート

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