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

HRID 991880

反応式

HRID 991880 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-92ff867ea2ef498bbbe1006bdae4a4e0
出典データセット
uspto-grants-2002_10
特許番号
US06465660B1

関連ノート

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