Benzonitrile → 2-Aminobenzothiazole-6-carbonitrile

HRID 9100

反応式

HRID 9100 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[S-:10][C:11]#[N:12].[K+].BrBr.C(#N)C1C=CC=CC=1>C(O)(=O)C.O>[NH2:12][C:11]1[S:10][C:3]2[CH:4]=[C:5]([C:6]#[N:7])[CH:8]=[CH:9][C:2]=2[N:1]=1

参加物

7

反応物 4

HCID 7505BenzonitrileHCID 133964-AminobenzonitrileHCID 24408BromineHCID 516872Potassium thiocyanate

生成物 1

HCID 43271392-Aminobenzothiazole-6-carbonitrile

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

実験手順

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.

後処理

  1. temperatureis cooled to about 16–30° C., preferably 16–18° C
  2. customthe flask is then equipped with an addition funnel
  3. filtrationfiltered
  4. washThe presscake is washed well with water
  5. filtrationfiltered
  6. washAgain the presscake is washed well with water

出典と根拠

ORDレコード
ord-6eca5615015f4ce68df2769bea908bce
出典データセット
uspto-grants-2006_08
特許番号
US07091227B2

関連ノート

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