Ammonia → 2-Propoxyaniline

HRID 67242

反応式

HRID 67242 の反応式
Cl.C(O)C.[CH2:5]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-])=O)[CH2:6][CH3:7].N>[Fe].O>[CH2:5]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[NH2:15])[CH2:6][CH3:7]

参加物

7

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 702EthanolHCID 5874971-Nitro-2-propoxybenzene

生成物 1

HCID 21134322-Propoxyaniline収率 74%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒

反応条件

温度
30 °C

実験手順

Iron 60 mesh (134.5 g., 2.40 mole), concentrated HCl (37.4 cc), ethanol (630 cc), and water (570 cc) are stirred under nitrogen and the temperature of the mixture is raised to reflux. Then o-propoxynitrobenzene (12.5 g., 0.69 mole), is added at reflux over a period of 5 hrs. and refluxed for 3-4 hrs. Then the mixture is neutralized with concentrated ammonia to a pH of 8-9. The temperature is raised to 30° C., and the reaction mass filtered, 200 cc ether added, the organic layer separated. The product distilled at vapor temperature of 65°-67° C. at 0.05-0.03 mm. yielding 77 g of product (74%).

後処理

  1. temperaturethe temperature of the mixture is raised
  2. temperatureto reflux
  3. temperatureat reflux over a period of 5 hrs
  4. temperatureand refluxed for 3-4 hrs
  5. filtrationthe reaction mass filtered
  6. addition200 cc ether added
  7. customthe organic layer separated
  8. distillationThe product distilled at vapor temperature of 65°-67° C. at 0.05-0.03 mm

出典と根拠

ORDレコード
ord-705d73ec38b3401f83c100f1fa09f482
出典データセット
uspto-grants-1982_08
特許番号
US04345937

関連ノート

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