تفاعل #41578

معادلة التفاعل

aniline

pyridine-2-carboxaldehyde

4-(2-chlorophenoxy)-5-(6-methanesulfonyl-pyridin-3-yloxy)-benzene-1,2-diamine

→

compound

5-(2-chloro-phenoxy)-2-pyridin-2-yl-6-(6-methanesulfonyl-pyridin-3-yloxy)-1H-benzimidazole

المذيبات

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىobtained in (step 1)
2. 2
   أخرىthe reaction liquid
3. 3
   أخرىThe solvent was evaporated away under reduced pressure
4. 4
   أخرىthe resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]
5. 5
   workup.ADDITIONThe solvent of the resulting fraction was diluted with ethyl acetate
6. 6
   غسيلwashed with aqueous saturated sodium bicarbonate
7. 7
   تجفيفdried with anhydrous sodium sulfate
8. 8
   أخرىThe solvent was evaporated away under reduced pressure

الإجراء التجريبي

0.26 ml of 1 M methanol solution of aniline and pyridine-2-carboxaldehyde (1/1) was added to a methanol (1 ml) solution of 35 mg of 4-(2-chlorophenoxy)-5-(6-methanesulfonyl-pyridin-3-yloxy)-benzene-1,2-diamine obtained in (step 1), and the reaction liquid was stirred overnight at 60° C. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid]. The solvent of the resulting fraction was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate, and then dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound as a pale yellow solid.

المصدر