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

HRID 1582175

反応式

HRID 1582175 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-940390aa431f436ea10b6d9f617a339c
出典データセット
uspto-grants-2004_05
特許番号
US06734198B1

関連ノート

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