تفاعل #483552

معادلة التفاعل

2-methylthio-4-iodopyrimidine

5Chloro-2-(4fluorophenyl)imidazo[4,5-b]pyridine

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title compound

المردود 71.1%

5-Chloro-2-(4-fluorophenyl)-1-(2-methylthio-4-pyrimidinyl)imidazo[4,5-b]pyridine

المردود 71.1%

المذيبات

toluene

toluene

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated for 20 h at 120° C
2. 2
   workup.ADDITIONThe reaction mixture is poured on water
3. 3
   استخلاصextracted with ethyl acetate three times
4. 4
   تجفيفThe combined organic phases are dried over Na2SO4
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated to dryness
7. 7
   أخرىto yield the crystalline crude product, which
8. 8
   أخرىafter recrystallisation from ethyl acetate

الإجراء التجريبي

KN(TMS)2 (1.42 g 7.16 mmol) in toluene (7 ml) is added at 0° C. to a solution of 5Chloro-2-(4fluorophenyl)imidazo[4,5-b]pyridine (1.9 g 6.66 mmol) in DMF (25 ml). After stirring 1 h at room temperature, 2-methylthio-4-iodopyrimidine (1.8 g 7.1 mmol) in toluene (7 ml) is added dropwise and heated for 20 h at 120° C. The reaction mixture is poured on water and extracted with ethyl acetate three times. The combined organic phases are dried over Na2SO4, filtered and evaporated to dryness to yield the crystalline crude product, which after recrystallisation from ethyl acetate yields the title compound as colorless crystals (1.76 g 67%).

المصدر