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

HRID 2175376ノート

反応式

HRID 2175376 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 198299443-((4-Methoxybenzyl)oxy)aniline収率 99.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 22242641Methanol--water (1/1)溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-04c51b389c0e4850b765aa9505c3d79a
出典データセット
uspto-grants-2015_06
特許番号
US09062066B2

反応ノート

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