تفاعل #2486769

ord-cfae78fceb714553a0b7edce08385c9b

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITION5 ml (0.053 mol) of boranedimethyl sulfide complex are added at 0° C
  2. 2
    غسيلthe mixture is washed with water
  3. 3
    تجفيفThe organic phase is dried over magnesium sulfate
  4. 4
    أخرىthe solvent is removed by distillation, and 9.23 g (98% of theory) of N-tert-butyl-2-methoxycarbonyl-5-methylaminobenzenesulfonamide
  5. 5
    أخرىare obtained

الإجراء التجريبي

9.92 g (0.032 mol) of N-tert-butyl-5-formylamino-2-methoxycarbonylbenzenesulfonamide are dissolved in 50 ml of CHCl3, and then 5 ml (0.053 mol) of boranedimethyl sulfide complex are added at 0° C. After 1 h at 0° C. and 3 h at room temperature the reaction mixture is cooled to 0° C. 30 ml of methanol are added and the mixture is washed with water. The organic phase is dried over magnesium sulfate, the solvent is removed by distillation, and 9.23 g (98% of theory) of N-tert-butyl-2-methoxycarbonyl-5-methylaminobenzenesulfonamide are obtained. m.p.: 120°-124° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05449812uspto-grants-1995_09