تفاعل #1946559

ord-25628e18afca447b9090904f78886bdc

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated on a steam bath for 22 hrs
  2. 2
    درجة الحرارةcooled
  3. 3
    أخرىThe water phase was decanted from the solid phase
  4. 4
    غسيلthe solid was washed with water and methanol
  5. 5
    أخرىRecrystallization of the solid from methanol

الإجراء التجريبي

To a mixture of 174.15 g (0.50 mol) of N,N-di-n-butyl-N′-(4-t-butylbenzoyl)thiourea (compound 1-2), 44.0 g (1.10 mol) of sodium hydroxide and 500 ml of water was added 56.70 g (0.60 mol) of chloroacetic acid. The mixture was stirred and heated on a steam bath for 22 hrs and cooled. The water phase was decanted from the solid phase, and the solid was washed with water and methanol. Recrystallization of the solid from methanol gave 85.6 g (49.7% yield) of product; mp: 48.5-49.5° C. The NMR spectrum was consistent with the proposed structure. Anal. Calcd. for C21H32N2S: C, 73.20; H, 9.36; N, 8.13; S, 9.30. Found: C, 73.04; H, 9.29; N, 8.02; S, 9.19.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06528223B1uspto-grants-2003_03