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

HRID 393592노트

반응식

HRID 393592 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 219910685-Benzyloxy-2-fluoro-4-methylaniline수율 100.1%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-cfc0ceaa331d4cb68eb0530bf25929f4
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06809097B1

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