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

HRID 2236570노트

반응식

HRID 2236570 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-bed74967eaa54242b39def900d23ad2f
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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