Ethanol → Ethyl 4-bromobenzene-1-carboximidate

HRID 1020939노트

반응식

HRID 1020939 반응식
[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]

참가 물질

3

반응물 2

HCID 702EthanolHCID 12162Benzonitrile, 4-bromo-

생성물 1

HCID 10466301Ethyl 4-bromobenzene-1-carboximidate

반응 조건

온도
2.5 °C

실험 절차

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.)

후처리

  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

출처 및 근거

ORD 기록
ord-3748fbfe636f4c7e8440745b1f7f7c83
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716483B2

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