Methanol → 3-((4-Methoxybenzyl)oxy)aniline

HRID 2175376노트

반응식

HRID 2175376 반응식
CO.O.[CH3:4][O:5][C:6]1[CH:22]=[CH:21][C:9]([CH2:10][O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-])=O)[CH:13]=2)=[CH:8][CH:7]=1>CO.O.[Fe]>[CH3:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH2:10][O:11][C:12]2[CH:13]=[C:14]([CH:15]=[CH:16][CH:17]=2)[NH2:18])=[CH:21][CH:22]=1

참가 물질

6

반응물 3

HCID 887MethanolHCID 962WaterHCID 36283881-[(4-Methoxyphenyl)Methoxy]-3-nitro-Benzene

생성물 1

HCID 198299443-((4-Methoxybenzyl)oxy)aniline수율 99.2%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 22242641Methanol--water (1/1)용매

실험 절차

Fe (5.6 g, 100.28 mmol) was mixed with methanol:H2O (15 ml:3 ml) and refluxed for 30 minutes. After the temperature is dropped to room temperature, 1-(4-methoxybenzyloxy)-3-nitrobenzene (1.3 g, 5.01 mmol) dissolved in 6 ml of methanol:H2O (5:1) was added and then refluxed for 15 hours. Fe was removed using cellite, then the reaction mixture was washed using methanol and concentrated under vacuum to remove the solvent. After extraction with 100 ml of saturated ammonium chloride+150 ml of dichloromethane, the organic layer was washed with water. The organic solvent was concentrated under vacuum to obtain the title compound (1.14 g, 99%).

후처리

  1. additionAfter the temperature is dropped to room temperature
  2. additionwas added
  3. temperaturerefluxed for 15 hours
  4. customFe was removed
  5. washthe reaction mixture was washed
  6. concentrationconcentrated under vacuum
  7. customto remove the solvent
  8. extractionAfter extraction with 100 ml of saturated ammonium chloride+150 ml of dichloromethane
  9. washthe organic layer was washed with water
  10. concentrationThe organic solvent was concentrated under vacuum

출처 및 근거

ORD 기록
ord-04c51b389c0e4850b765aa9505c3d79a
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09062066B2

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