반응 #61879

반응 방정식

Water

chlorosulfonyl isocyanate

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

hydrochloric acid

→

title compound

N-(4,6-dimethyl-1-octyl-5-ureidoindolin-7-yl)-2,2-dimethylpropanamide hydrochloride

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred at room temperature for 30 min
2. 2
   추출the mixture was extracted with chloroform (100 mL)
3. 3
   세척The chloroform layer was washed with saturated brine
4. 4
   건조dried over sodium sulfate
5. 5
   기타Chloroform was evaporated under reduced pressure
6. 6
   기타the obtained crystalline residue was recrystallized from a mixture of chloroform-diisopropyl ether

실험 절차

N-(5-Amino-4,6-dimethyl-1-octylindolin-7-yl)-2,2-dimethylpropanamide (500 mg) was dissolved in methylene chloride (5.0 mL), and chlorosulfonyl isocyanate (0.14 mL) was added dropwise at −60° C. The mixture was stirred at the same temperature for 3 hr and 6M hydrochloric acid (0.45 mL) was added. The mixture was stirred at room temperature for 30 min. Water (50 mL) was added to the reaction solution and the mixture was extracted with chloroform (100 mL). The chloroform layer was washed with saturated brine and dried over sodium sulfate. Chloroform was evaporated under reduced pressure and the obtained crystalline residue was recrystallized from a mixture of chloroform-diisopropyl ether to give the title compound as crystals (407 mg).

출처