تفاعل #45813

معادلة التفاعل

sodium hydroxide

N-iodosuccinimide

4-Amino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]biphenyl-3-carbonitrile

chloroform

→

compound

المردود 63.0%

4-Amino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-5-iodobiphenyl-3-carbonitrile

المردود 63.0%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   أخرىthe reaction liquid
2. 2
   غسيلThe organic layer was washed with saturated brine
3. 3
   تجفيفdried over anhydrous sodium sulfate
4. 4
   أخرىThe insoluble matter was separated by filtration
5. 5
   أخرىthe solvent was evaporated away
6. 6
   أخرىthe resulting residue was purified by preparative TLC (eluent, chloroform:methanol=9:1)

الإجراء التجريبي

4-Amino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]biphenyl-3-carbonitrile (I-243) (75 mg, 0.25 mmol) was dissolved in acetic acid (1 ml), and at room temperature, N-iodosuccinimide (66 mg, 0.29 mmol) was added. After stirring under nitrogen atmosphere at the same temperature for 6 hours, the reaction liquid was fractionated with chloroform and aqueous 1 M sodium hydroxide solution. The organic layer was washed with saturated brine, then dried over anhydrous sodium sulfate. The insoluble matter was separated by filtration, the solvent was evaporated away, and the resulting residue was purified by preparative TLC (eluent, chloroform:methanol=9:1) to obtain the entitled compound (67 mg, 63%) as a brown gel.

المصدر