Hydrazine hydrate (1:1) → 1-Propyl-2,3-dihydro-1h-indol-5-ylamine

HRID 352336

반응식

HRID 352336 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[N:9]([CH2:13][CH2:14][CH3:15])[CH2:8][CH2:7]2)([O-])=O.O.NN>[Ni].C(O)C>[CH2:13]([N:9]1[C:10]2[C:6](=[CH:5][C:4]([NH2:1])=[CH:12][CH:11]=2)[CH2:7][CH2:8]1)[CH2:14][CH3:15]

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 98342765-Nitro-1-propylindoline

생성물 1

HCID 98775221-Propyl-2,3-dihydro-1h-indol-5-ylamine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

Approximately 400 mg of Raney nickel is added to a mixture of 3.28 g (15.9 mmol) of 5-nitro-1-propylindoline and 4 ml (80 mmol) of hydrazine hydrate in 60 ml of absolute ethanol. The reaction mixture is heated under reflux for 5 hours. After returning to 23° C., a little silica is added to the flask and the solvent is evaporated off under vacuum. The evaporation residue is placed directly at the top of a chromatography column. The expected product is eluted using a Heptane/AcOEt mixture (1/9). A black oil is obtained which is used directly in the following stage.

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux for 5 hours
  3. customAfter returning to 23° C.
  4. additiona little silica is added to the flask
  5. customthe solvent is evaporated off under vacuum
  6. washThe expected product is eluted
  7. customA black oil is obtained which

출처 및 근거

ORD 기록
ord-0e47d5ac8b3e4373b32d65814e1f0990
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06747024B1

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