반응 #61876

반응 방정식

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

용매

Methylene chloride

methylene chloride

triethylamine

반응 조건

후처리

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

실험 절차

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).

출처