Ethanol → Ethyl 4-bromobenzene-1-carboximidate

HRID 1020939

反応式

HRID 1020939 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[CH3:10][CH2:11][OH:12]>>[CH2:11]([O:12][C:6](=[NH:7])[C:5]1[CH:8]=[CH:9][C:2]([Br:1])=[CH:3][CH:4]=1)[CH3:10]

参加物

3

反応物 2

HCID 702EthanolHCID 12162Benzonitrile, 4-bromo-

生成物 1

HCID 10466301Ethyl 4-bromobenzene-1-carboximidate

反応条件

温度
2.5 °C

実験手順

4-Bromo-benzonitrile (5 g) was suspended in absolute EtOH (100 ml) and cooled to 0-5° C. HCl gas was bubbled through, initially vigorously for several minutes and later slowly for 5 hours. The resulting solution was allowed to stir overnight. Most of solvent was removed and the precipitate was filtered, washed with EtOH twice and dried to afford compound 2BN (4.1 g) as white solid. (Note: large scale synthesis may take longer time to get reaction complete. It is better to monitor the disappearance of starting material to get reaction end point.)

後処理

  1. customHCl gas was bubbled through, initially vigorously for several minutes
  2. customMost of solvent was removed
  3. filtrationthe precipitate was filtered
  4. washwashed with EtOH twice
  5. customdried
  6. customto afford compound 2BN (4.1 g) as white solid
  7. custom(Note: large scale synthesis
  8. customto get
  9. customreaction complete
  10. customto get
  11. customreaction end point

出典と根拠

ORDレコード
ord-3748fbfe636f4c7e8440745b1f7f7c83
出典データセット
uspto-grants-2014_05
特許番号
US08716483B2

関連ノート

読み込み中…