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

HRID 856055노트

반응식

HRID 856055 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 694813093-(4-Trifluoromethylphenyl)-2-propenylamine수율 100.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-32f9446a45494c429fb93c407919d778
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262212B2

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