تفاعل #68768

ord-633ce97e39b945cbbbe4136863d78fed

الكواشف

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solid materials formed
  2. 2
    ترشيحwere filtered off
  3. 3
    غسيلthe filtrate was washed with 1 M HCl (1 ml)
  4. 4
    تجفيفThe organic phase was dried over MgSO4
  5. 5
    أخرىevaporated in vacuum
  6. 6
    أخرىto give 0.4 g of CT corresponding to a yield of 87%

الإجراء التجريبي

DCC coupling reaction was used to couple the carboxylic group of chlorambucil with the hydroxyl group of TEMPOL with the loss of a water molecule. To a stirred solution of TEMPOL (0.172 g, 1 mmol) and chlorambucil (0.304 g, 1 mmol) in methylene chloride (5 ml) at 0° C. under argon, DCC (0.206 g, 1 mmol) (Dicyclohexyl carbodiimide) and DMAP (0.0307 g, 0.25 mmol) (Dimethyl amino pyridine) were added and the reaction mixture was stirred for 12 hrs at room temperature. The solid materials formed were filtered off, and the filtrate was washed with 1 M HCl (1 ml) followed by saturated NaHCO3 (2 ml) and brine (2 ml). The organic phase was dried over MgSO4 and evaporated in vacuum to give 0.4 g of CT corresponding to a yield of 87%. TLC (Thin Layer Chromatography) of the product showed a single spot only.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530434B2uspto-grants-2013_09