Chlorosuccinimide → 5-Chloro-2-(3,4,4-trifluoro-3-butenylthio)thiazole

HRID 1582175노트

반응식

HRID 1582175 반응식
[F:1][C:2](=[C:11]([F:13])[F:12])[CH2:3][CH2:4][S:5][C:6]1[S:7][CH:8]=[CH:9][N:10]=1.[Cl:14]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Cl:14][C:8]1[S:7][C:6]([S:5][CH2:4][CH2:3][C:2]([F:1])=[C:11]([F:12])[F:13])=[N:10][CH:9]=1

참가 물질

4

반응물 2

HCID 31398ChlorosuccinimideHCID 11447455Thiazole, 2-[(3,4,4-trifluoro-3-butenyl)thio]-

생성물 1

HCID 112307045-Chloro-2-(3,4,4-trifluoro-3-butenylthio)thiazole

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

2-(3,4,4-Trifluoro-3-butenylthio)thiazole (6.75 g, 30 mM) is dissolved in carbon tetrachloride (60 ml). N-chlorosuccinimide (4.8 g) is added to the solution and refluxed for 18 hours by heating. As soon as the reaction has reached room temperature, the mixture is filtered and the solvent is distilled off. The concentrate is purified by column chromatography (eluent: hexane/ethyl acetate=90/10) to obtain 5-chloro-2-(3,4,4-trifluoro-3-butenylthio)thiazole as pale yellow liquid (n20D 1.5326).

후처리

  1. temperaturerefluxed for 18 hours
  2. temperatureby heating
  3. customhas reached room temperature
  4. filtrationthe mixture is filtered
  5. distillationthe solvent is distilled off
  6. customThe concentrate is purified by column chromatography (eluent: hexane/ethyl acetate=90/10)

출처 및 근거

ORD 기록
ord-940390aa431f436ea10b6d9f617a339c
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06734198B1

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