반응 #9263

ord-d0a3bdf85e9b4840981acc50d0208080

반응 방정식

N#Cc1ccccc1
benzonitrile
N#C[S-].[K+]
potassium thiocyanate
N#Cc1ccc(N)cc1
4-aminobenzonitrile
BrBr
bromine
N#CCc1ccc2nc(N)sc2c1
(2-Amino-1,3-benzothiazol-6-yl)methyl cyanide

반응 조건

온도
16°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the flask is equipped with an addition funnel
  2. 2
    여과filtered
  3. 3
    세척The presscake is washed well with water
  4. 4
    여과filtered
  5. 5
    세척Again the presscake is washed well with water
  6. 6
    기타After drying in vacuo
  7. 7
    기타about 2 grams is isolated

실험 절차

2 grams of 4-aminobenzonitrile is dissolved in about 40 mL acetic acid and the solution is cooled to about 16° C. About 3.3 g of potassium thiocyanate is added and the flask is equipped with an addition funnel. The addition funnel is charged with about 2.7 g bromine and about 5 ml 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 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. After drying in vacuo, about 2 grams is isolated.

출처

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