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

HRID 9167

反応式

HRID 9167 の反応式
[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

参加物

7

反応物 4

HCID 7505BenzonitrileHCID 133964-AminobenzonitrileHCID 24408BromineHCID 516872Potassium thiocyanate

生成物 1

HCID 21298164(2-Amino-1,3-benzothiazol-6-yl)acetonitrile

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
16 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d0a3bdf85e9b4840981acc50d0208080
出典データセット
uspto-grants-2006_08
特許番号
US07091227B2

関連ノート

読み込み中…