تفاعل #45833

معادلة التفاعل

pivaloyl chloride

chloroform

4,5-diamino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methylbiphenyl-3-carbonitrile

→

compound

المردود 43.0%

N-[4-Amino-5-cyano-2-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-methylbiphenyl-3-yl]-2,2-dimethylpropionamide

المردود 43.0%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   أخرىthe reaction
2. 2
   استخلاصfollowed by extraction with chloroform
3. 3
   غسيلThe organic layer was washed with an aqueous saturated sodium hydrogencarbonate solution and saturated brine
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   أخرىThe solvent was evaporated away under reduced pressure
6. 6
   غسيلeluted with a mixed solvent of chloroform/methanol (95:5

الإجراء التجريبي

With cooling with ice, pivaloyl chloride (0.46 ml, 3.73 mmol) was dropwise added to a chloroform (40 ml) solution of 4,5-diamino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methylbiphenyl-3-carbonitrile (I-269) (1.25 g, 3.73 mmol). After stirring for 3 hours, water was added to the reaction liquid to stop the reaction, followed by extraction with chloroform. The organic layer was washed with an aqueous saturated sodium hydrogencarbonate solution and saturated brine, then dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, then the residue was subjected to column chromatography, and eluted with a mixed solvent of chloroform/methanol (95:5, v/v) to obtain the entitled compound (675 mg, 43%) as a brown amorphous substance.

المصدر