Hydrazine hydrate (1:1) → (E)-(2-chloro-4-(3-(3,5-dichlorophenyl)-4,4,4-trifluorobut-1-en-1-yl)phenyl)methanamine

HRID 1502718노트

반응식

HRID 1502718 반응식
[Cl:1][C:2]1[CH:19]=[C:18](/[CH:20]=[CH:21]/[CH:22]([C:27]2[CH:32]=[C:31]([Cl:33])[CH:30]=[C:29]([Cl:34])[CH:28]=2)[C:23]([F:26])([F:25])[F:24])[CH:17]=[CH:16][C:3]=1[CH2:4][N:5]1C(=O)C2C(=CC=CC=2)C1=O.O.NN>CCO>[Cl:1][C:2]1[CH:19]=[C:18](/[CH:20]=[CH:21]/[CH:22]([C:27]2[CH:28]=[C:29]([Cl:34])[CH:30]=[C:31]([Cl:33])[CH:32]=2)[C:23]([F:25])([F:26])[F:24])[CH:17]=[CH:16][C:3]=1[CH2:4][NH2:5]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 86675180(E)-2-(2-chloro-4-(3-(3,5-dichlorophenyl)-4,4,4-trifluorobut-1-en-1-yl)benzyl)isoindoline-1,3-dione

생성물 1

HCID 86675181(E)-(2-chloro-4-(3-(3,5-dichlorophenyl)-4,4,4-trifluorobut-1-en-1-yl)phenyl)methanamine수율 100%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

To a stirred solution of (E)-2-(2-chloro-4-(3-(3,5-dichlorophenyl)-4,4,4-trifluorobut-1-en-1-yl)benzyl)isoindoline-1,3-dione (0.4 g, 0.76 mmol) in EtOH was added hydrazine hydrate (0.38 g, 7.6 mmol), and the resultant reaction mixture was heated at 80° C. for 2 h. The reaction mixture was filtered, and the filtrate was concentrated. The residue was dissolved in CH2Cl2, washed with brine, dried over Na2SO4, and concentrated under reduced pressure to afford the title compound as a gummy liquid (0.3 g), which was carried on to the next step without further purification.

후처리

  1. customthe resultant reaction mixture
  2. filtrationThe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe residue was dissolved in CH2Cl2
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7e136ef187bd4ac19d14ca606c795b3a
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09210927B2

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