تفاعل #61876

معادلة التفاعل

Methanol

chlorosulfonyl isocyanate

N-(5-Amino-4,6-dimethyl-1-octylindolin-7-yl)-2,2-dimethylpropanamide

→

title compound

N-[5-(N-methoxycarbonylsulfamoylamino)-4,6-dimethyl-1-octylindolin-7-yl]-2,2-dimethylpropanamide

المذيبات

Methylene chloride

methylene chloride

triethylamine

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added at −20° C
2. 2
   workup.STIRRINGthe mixture was further stirred at −9° C. for 30 min
3. 3
   غسيلthe mixture was washed successively with 10% aqueous citric acid, saturated aqueous sodium hydrogencarbonate and saturated brine
4. 4
   تجفيفdried over sodium sulfate
5. 5
   أخرىMethylene chloride was evaporated under reduced pressure
6. 6
   أخرىThe obtained residue was purified by silica gel column chromatography

الإجراء التجريبي

Methanol (0.13 mL) was added to methylene chloride (2.6 mL) and chlorosulfonyl isocyanate (0.29 mL) was added at −20° C. The mixture was stirred at −20° C. to 10° C. for 20 min. N-(5-Amino-4,6-dimethyl-1-octylindolin-7-yl)-2,2-dimethylpropanamide (612 mg) and triethylamine (0.46 mL) were added to the reaction mixture and the mixture was further stirred at −9° C. for 30 min. Methylene chloride was added to the reaction mixture, and the mixture was washed successively with 10% aqueous citric acid, saturated aqueous sodium hydrogencarbonate and saturated brine and dried over sodium sulfate. Methylene chloride was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as crystals. (601 mg).

المصدر