تفاعل #53575

معادلة التفاعل

2-(2,2,2-trifluoroethylthio)-4-(3-trifluoromethylpyrazolyl)benzaldehyde

dioxane

potassium carbonate

→

[2-ethenyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide

المردود 43.8%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwith heating for 5 hours
2. 2
   ترشيحthe insolubles were filtered off
3. 3
   workup.DISTILLATIONthe dioxane was distilled off under reduced pressure
4. 4
   أخرىPurification of the residue by silica gel column chromatography

الإجراء التجريبي

2.83 g (8.0 mmol) of 2-(2,2,2-trifluoroethylthio)-4-(3-trifluoromethylpyrazolyl)benzaldehyde (Compound No. V-275 of the present invention) prepared in the same manner as in Example 8 (9), 2.85 g (8.0 mmol) of methyltriphenylphosphonium bromide and 1.38 g (10.0 mmol) of potassium carbonate were refluxed in a solvent mixture of 20 ml of dioxane and 0.3 ml of water with heating for 5 hours. After cooling down to room temperature, the insolubles were filtered off, and the dioxane was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.23 g of [2-ethenyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide (yield 43.8%) as a pale yellow liquid (nD20 1.5328).

المصدر