Hydrazine hydrate (1:1) → 5-Benzyloxy-2-fluoro-4-methylaniline

HRID 393592

反応式

HRID 393592 の反応式
[CH2:1]([O:8][C:9]1[C:10]([CH3:19])=[CH:11][C:12]([F:18])=[C:13]([N+:15]([O-])=O)[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN>CO.[Ni]>[CH2:1]([O:8][C:9]1[C:10]([CH3:19])=[CH:11][C:12]([F:18])=[C:13]([CH:14]=1)[NH2:15])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 219910575-Benzyloxy-2-fluoro-4-methylnitrobenzene

生成物 1

HCID 219910685-Benzyloxy-2-fluoro-4-methylaniline収率 100.1%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒2 回

実験手順

5-Benzyloxy-2-fluoro-4-methyl-1-nitrobenzene (500 mg, 1.9 mmol) in methanol (110 ml) was added to a suspension of Raney nickel (75 mg) and hydrazine hydrate (0.47 ml, 9.5 mmol) in methanol (10 ml) and heated at reflux. The mixture was maintained under reflux for 15 minutes and then the insoluble materials removed by filtration through diatomaceous earth. The filter pad was washed with methanol and the solvent removed from the filtrate by evaporation to give 5-benzyloxy-2-fluoro-4-methylaniline (440 mg, 99%).

後処理

  1. temperatureheated
  2. temperatureat reflux
  3. temperatureThe mixture was maintained
  4. temperatureunder reflux for 15 minutes
  5. customthe insoluble materials removed by filtration through diatomaceous earth
  6. washThe filter pad was washed with methanol
  7. customthe solvent removed from the filtrate by evaporation

出典と根拠

ORDレコード
ord-cfc0ceaa331d4cb68eb0530bf25929f4
出典データセット
uspto-grants-2004_10
特許番号
US06809097B1

関連ノート

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