تفاعل #7024

معادلة التفاعل

chloroform

5-[5-(3-Methoxypropyl)-1,3,4-oxadiazol-2-yl]-2-phenylpyridine

3-amino-2-methylbenzamide

D-10-camphorsulfonic acid

→

compound

المردود 56.1%

3-[3-(3-Methoxypropyl)-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-4-yl]-2-methylbenzamide

المردود 56.1%

المذيبات

1,3-dimethyl-2-imidazolidinone

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter the reaction solution was cooled to ambient temperature
2. 2
   غسيلwas then washed with saturated aqueous sodium hydrogen carbonate solution
3. 3
   تجفيفThe organic layer was dried over anhydrous magnesium sulfate
4. 4
   أخرىthe solvent was evaporated under reduced pressure
5. 5
   أخرىThe resulting residue was purified by silica gel column chromatography (eluent: chloroform/methanol=10/1)

الإجراء التجريبي

5-[5-(3-Methoxypropyl)-1,3,4-oxadiazol-2-yl]-2-phenylpyridine (1.0 g) prepared in the Reference Example 7 was dissolved in 1,3-dimethyl-2-imidazolidinone (10 ml), followed by addition of 3-amino-2-methylbenzamide (1.53 g) prepared in the Reference Example 6 and D-10-camphorsulfonic acid (290 mg), and stirred at 200° C. for 16 hours. After the reaction solution was cooled to ambient temperature, chloroform was added to the solution, which was then washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: chloroform/methanol=10/1), to afford the entitled compound (812 mg, 56%). The physico-chemical values are as follows.

المصدر