تفاعل #534192

معادلة التفاعل

1-(5,7-diiodo-benzothiazol-2-yl)-3-ethyl-urea

2-tributylstannyl-pyrazine

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title compound

1-(5,7-Di-pyrazin-2-yl-benzothiazol-2-yl)-3-ethyl-urea

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction mixture was degassed for half an hour
2. 2
   أخرىThe reaction mixture was again degassed for half an hour
3. 3
   أخرىAfter the completion of the reaction (TLC monitoring), DMF
4. 4
   workup.DISTILLATIONwas distilled off
5. 5
   workup.ADDITIONadded water
6. 6
   استخلاصextracted with ethyl acetate (×3)
7. 7
   تجفيفThe combined organic layer was dried over anhydrous Na2SO4
8. 8
   أخرىevaporated to dryness under reduced pressure
9. 9
   أخرىThe compound was purified by chromatography on silica (230-400 M)

الإجراء التجريبي

To a solution of 1-(5,7-diiodo-benzothiazol-2-yl)-3-ethyl-urea (0.50 g, 1.0 mmol) in DMF (5.0 mL) was added 2-tributylstannyl-pyrazine (0.78 g, 2.0 mmol) under nitrogen atmosphere at room temperature. The reaction mixture was degassed for half an hour followed by the addition of tetrakis(triphenylphosphine)palladium(0) (0.18 g, 0.10 mmol). The reaction mixture was again degassed for half an hour and then heated at 120° C. for 2 h under nitrogen atmosphere. After the completion of the reaction (TLC monitoring), DMF was distilled off, added water and extracted with ethyl acetate (×3). The combined organic layer was dried over anhydrous Na2SO4, and evaporated to dryness under reduced pressure. The compound was purified by chromatography on silica (230-400 M) using ethyl acetate/Methanol) (95:5) to provide the title compound as off white solid (0.025 g, 6.5%).

المصدر