N-bromobutanimide → 3-Bromo-5,6-dimethoxy-phthalide

HRID 991880

반응식

HRID 991880 반응식
[Br:1]N1C(=O)CCC1=O.[CH3:9][O:10][C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][C:20]=1[O:21][CH3:22])[C:16](=[O:17])[O:15][CH2:14]2>ClCCl>[Br:1][CH:14]1[C:13]2[C:18](=[CH:19][C:20]([O:21][CH3:22])=[C:11]([O:10][CH3:9])[CH:12]=2)[C:16](=[O:17])[O:15]1

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 2304605,6-Dimethoxy-3H-isobenzofuran-1-one

생성물 1

HCID 111965723-Bromo-5,6-dimethoxy-phthalide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

12 mmol of N-bromosuccinimide are added to 10 mmol of 5,6-dimethoxyphthalide dissolved in dichloromethane and then the reaction mixture, illuminated with a halogen lamp, is heated at reflux for 5 hours. The mixture is then brought to ambient temperature and filtered, and the filtrate is subsequently evaporated, toluene is added, the suspension obtained is filtered and the filtrate is evaporated. The residue obtained is filtered through silica to yield the expected product.

후처리

  1. customthe reaction mixture, illuminated with a halogen lamp
  2. temperatureis heated
  3. temperatureat reflux for 5 hours
  4. customis then brought to ambient temperature
  5. filtrationfiltered
  6. customthe filtrate is subsequently evaporated
  7. additiontoluene is added
  8. customthe suspension obtained
  9. filtrationis filtered
  10. customthe filtrate is evaporated
  11. customThe residue obtained
  12. filtrationis filtered through silica

출처 및 근거

ORD 기록
ord-92ff867ea2ef498bbbe1006bdae4a4e0
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06465660B1

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