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

HRID 1582176

반응식

HRID 1582176 반응식
[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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 663334-Bromo-1,1,2-trifluorobut-1-eneHCID 178527881HCID 178527881, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e2b8f333808345b8859dc34c25388125
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06734198B1

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