تفاعل #61879

ord-97faa260617b47e7aceb3f11cb388ad3

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07429612B2uspto-grants-2008_09