반응 #9196

ord-6eca5615015f4ce68df2769bea908bce

반응 방정식

N#Cc1ccccc1
benzonitrile
N#C[S-].[K+]
Potassium thiocyanate
N#Cc1ccc(N)cc1
4-Aminobenzonitrile
BrBr
bromine
N#Cc1ccc2nc(N)sc2c1
title compound
N#Cc1ccc2nc(N)sc2c1
2-Amino-1,3-benzothiazole-6-carbonitrile

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도is cooled to about 16–30° C., preferably 16–18° C
  2. 2
    기타the flask is then equipped with an addition funnel
  3. 3
    여과filtered
  4. 4
    세척The presscake is washed well with water
  5. 5
    여과filtered
  6. 6
    세척Again the presscake is washed well with water

실험 절차

4-Aminobenzonitrile is dissolved in acetic acid (or a weak protic acid) and the solution is cooled to about 16–30° C., preferably 16–18° C. Potassium thiocyanate is added and the flask is then equipped with an addition funnel. The addition funnel is charged with bromine and acetic acid. This dark solution is then added to the benzonitrile solution in a dropwise fashion under good agitation and allowed to stir for about 12–20 hours, preferrably about 16 hours. The slurry is then drowned into water and filtered. The presscake is washed well with water, reslurried in dilute aqueous alkali and filtered. Again the presscake is washed well with water to obtain the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091227B2uspto-grants-2006_08