Pyridine → 3-hydroxy-4-(2-methoxyethoxy)benzaldehyde O-methyloxime

HRID 2236570ノート

反応式

HRID 2236570 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[O:10][CH2:11][CH2:12][O:13][CH3:14])[CH:5]=O.CC[O:17][CH2:18]C.[N:20]1C=CC=CC=1>CCO>[CH3:18][O:17][N:20]=[CH:5][C:4]1[CH:7]=[CH:8][C:9]([O:10][CH2:11][CH2:12][O:13][CH3:14])=[C:2]([OH:1])[CH:3]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 3283Diethyl EtherHCID 426255193-Hydroxy-4-(2-methoxyethoxy)benzaldehyde

生成物 1

HCID 722508733-hydroxy-4-(2-methoxyethoxy)benzaldehyde O-methyloxime収率 81%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

An amount of 3-hydroxy-4-(2-methoxyethoxy)benzaldehyde (1.24 g, 6.32 mmol) in 20 mL of EtOH and 10 mL of pyridine is added methoxy]amine hydrochloride (1.06 g, 12.64 mmol). The reaction mixture is stirred at room temperature over weekend. Solvent is removed under vacuum to give colorless oil which is added ether, washed twice with saturated NaHCO3 solution, once with brine, dried over Mg2SO4, filtered and evaporated to give colorless oil. Leaving this oil overnight at room temperature gave 1.15 g (81.0% yield) of colorless solid: mp: 63-64° C.; MS (ESI) m/z 226.1 (M+H)+1

後処理

  1. customSolvent is removed under vacuum
  2. customto give colorless oil which
  3. washwashed twice with saturated NaHCO3 solution, once with brine
  4. dry with materialdried over Mg2SO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give colorless oil
  8. customLeaving this oil overnight at room temperature

出典と根拠

ORDレコード
ord-bed74967eaa54242b39def900d23ad2f
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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