Benzonitrile → (2-Amino-1,3-benzothiazol-6-yl)acetonitrile

HRID 9167

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HRID 9167 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#N)=[CH:4][CH:3]=1.[S-:10][C:11]#[N:12].[K+].BrBr.[C:16](#[N:23])C1C=CC=CC=1>C(O)(=O)C.O>[NH2:12][C:11]1[S:10][C:3]2[CH:4]=[C:5]([CH2:6][C:16]#[N:23])[CH:8]=[CH:9][C:2]=2[N:1]=1

참가 물질

7

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온도
16 °C

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.

후처리

  1. customthe flask is equipped with an addition funnel
  2. filtrationfiltered
  3. washThe presscake is washed well with water
  4. filtrationfiltered
  5. washAgain the presscake is washed well with water
  6. customAfter drying in vacuo
  7. customabout 2 grams is isolated

출처 및 근거

ORD 기록
ord-d0a3bdf85e9b4840981acc50d0208080
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091227B2

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