Potassium Carbonate → Thiazole, 2-[(3,4,4-trifluoro-3-butenyl)thio]-

HRID 1582176

反応式

HRID 1582176 の反応式
[SH:1][C:2]1[S:3][CH:4]=[CH:5][N:6]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:13]([C:16]([F:20])=[C:17]([F:19])[F:18])[CH2:14]Br>C(#N)C>[F:20][C:16](=[C:17]([F:19])[F:18])[CH2:13][CH2:14][S:1][C:2]1[S:3][CH:4]=[CH:5][N:6]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 663334-Bromo-1,1,2-trifluorobut-1-eneHCID 178527881HCID 178527881、化合物

生成物 1

HCID 11447455Thiazole, 2-[(3,4,4-trifluoro-3-butenyl)thio]-収率 86.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2-Mercaptothiazole (5.18 g), potassium carbonate (6.72 g) and 4-bromo-1,1,2-trifluorobutene-1 (9.21 g) are refluxed in acetonitrile (60 ml) in the presence of argon gas for 6 hours by heating. After the reaction mixture has reached room temperature, it is filtered and the solvent is distilled off. The residue is dissolved in dichloromethane and washed with 5% aqueous solution of sodium hydroxide and water in this order. It is dried over unhydrous sodium sulfate and purified by column chromatography (eluent: dichloromethane) to obtain 2-(3,4,4-trifluoro-3-butenyl-thio)thiazole (8.6 g) as pale yellow liquid (n20D 1.5200).

後処理

  1. temperatureby heating
  2. customhas reached room temperature
  3. filtrationit is filtered
  4. distillationthe solvent is distilled off
  5. dissolutionThe residue is dissolved in dichloromethane
  6. washwashed with 5% aqueous solution of sodium hydroxide and water in this order
  7. dry with materialIt is dried over unhydrous sodium sulfate
  8. custompurified by column chromatography (eluent: dichloromethane)

出典と根拠

ORDレコード
ord-e2b8f333808345b8859dc34c25388125
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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