Hydrazine hydrate (1:1) → 3-(4-Trifluoromethylphenyl)-2-propenylamine

HRID 856055ノート

反応式

HRID 856055 の反応式
[F:1][C:2]([F:24])([F:23])[C:3]1[CH:8]=[CH:7][C:6]([CH:9]=[CH:10][CH2:11]C23C=CC=CC2C(NC3=O)=O)=[CH:5][CH:4]=1.O.[NH2:26]N>C(O)C>[F:1][C:2]([F:24])([F:23])[C:3]1[CH:8]=[CH:7][C:6]([CH:9]=[CH:10][CH2:11][NH2:26])=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 694807362-[3-(4-Trifluoromethylphenyl)-2-propenyl]phthalimide

生成物 1

HCID 694813093-(4-Trifluoromethylphenyl)-2-propenylamine収率 100.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-[3-(4-trifluoromethylphenyl)-2-propenyl]phthalimide (4.57 g, 13.79 mmol) prepared in Reference Example 102 and hydrazine hydrate (897 mg, 17.93 mmol) in ethanol (80 ml) was heated under reflux for 3 hours. The reaction mixture was allowed to return to room temperature and filtered, and the filtrate was concentrated under reduced pressure. To the residue, ethyl acetate was added, and the resulting mixture was washed with 1 N sodium hydroxide aqueous solution and brine, and dried over magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure to afford 3-(4-trifluoromethylphenyl)-2-propenylamine (2.78 g, quantitative) as a pale brown crystalline powder.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. customto return to room temperature
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionTo the residue, ethyl acetate was added
  7. washthe resulting mixture was washed with 1 N sodium hydroxide aqueous solution and brine
  8. dry with materialdried over magnesium sulfate
  9. filtrationAfter filtration
  10. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-32f9446a45494c429fb93c407919d778
出典データセット
uspto-grants-2007_08
特許番号
US07262212B2

反応ノート

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