Formaldehyde → HCID 69433836、化合物

HRID 1294453ノート

反応式

HRID 1294453 の反応式
Cl.[C:2]([C:4]1[CH:12]=[CH:11][C:7]([CH2:8][O:9][NH2:10])=[C:6]([O:13][CH2:14][CH3:15])[CH:5]=1)#[N:3].[CH3:16][OH:17].C=O>O>[C:2]([C:4]1[CH:12]=[CH:11][C:7]([CH2:8][O:9][NH2:10])=[C:6]([O:13][CH2:14][CH3:15])[CH:5]=1)#[N:3].[CH2:16]=[O:17]

参加物

5

反応物 3

HCID 712FormaldehydeHCID 887MethanolHCID 69434226O-(4-cyano-2-ethoxybenzyl)hydroxyamine hydrochloride

生成物 1

HCID 69433836HCID 69433836、化合物収率 96%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

O-(4-cyano-2-ethoxybenzyl)hydroxyamine hydrochloride (19-1, 2.7 g, 0.012 mol), methanol (20 ml) and water (20 ml) were charged, and a 36% formaldehyde aqueous solution was added to this, and the mixture was stirred at room temperature for 2.0 hours. Water was added to the mixture and the mixture was extracted with ethyl acetate. The resulted ethyl acetate layer was dried over anhydrous magnesium sulfate, then, the solvent was distilled off under reduce pressure. This was purified by silica gel column chromatography using hexane/ethyl acetate system, to obtain O-(4-cyano-2-ethoxybenzyl)hydroxyamine-formaldehyde derivative (3-1a, 2.2 g, yield 96%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe resulted ethyl acetate layer was dried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off
  4. customThis was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-b635086fdb4b4c5d979b53b05dc73ddb
出典データセット
uspto-grants-2007_07
特許番号
US07241625B2

反応ノート

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