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

HRID 352336

反応式

HRID 352336 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0e47d5ac8b3e4373b32d65814e1f0990
出典データセット
uspto-grants-2004_06
特許番号
US06747024B1

関連ノート

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