تفاعل #465448

ord-3d86680f96b441e0a962cb5deb85622f

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONtreated in an ultra-sound bath for 15 minutes
  2. 2
    ترشيحThe precipitate was filtered off
  3. 3
    workup.DISSOLUTIONdissolved in 10 ml of 0.1N NaOH
  4. 4
    ترشيحfiltered
  5. 5
    ترشيحThe precipitate was filtered off under suction
  6. 6
    غسيلwashed with water
  7. 7
    أخرىdried

الإجراء التجريبي

0.314 g (0.001 mol) of 4-amino-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide and 6.6 ml (0.1 mol) of ethylamine were stirred in 15 ml of ethanol in an autoclave at 130° C. for 3 hours. The reaction mixture was freed from solvent, the residue was suspended in 8 ml of ethanol and treated in an ultra-sound bath for 15 minutes. The precipitate was filtered off, dissolved in 10 ml of 0.1N NaOH and filtered. The filtrate was adjusted to pH 6 with 01N HCl. The precipitate was filtered off under suction, washed with water and dried. There was obtained 0.18 g (56%) of 4-amino-N-(6-ethylamino-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide as white crystals; m.p.: 252° C. (dec.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06030976uspto-grants-2000_02