Pyridine → 1-Methyl-4-bromoacetyl-5-(2-fluorobenzoyl)-1,2,3,4-tetrahydroquinoxaline

HRID 1109721ノート

反応式

HRID 1109721 の反応式
[CH3:1][N:2]1[C:11]2[C:6](=[C:7]([C:12](=[O:20])[C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])[CH:8]=[CH:9][CH:10]=2)[NH:5][CH2:4][CH2:3]1.N1C=CC=CC=1.[Br:27][CH2:28][C:29](Br)=[O:30]>C(Cl)Cl>[CH3:1][N:2]1[C:11]2[C:6](=[C:7]([C:12](=[O:20])[C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])[CH:8]=[CH:9][CH:10]=2)[N:5]([C:29](=[O:30])[CH2:28][Br:27])[CH2:4][CH2:3]1

参加物

5

反応物 3

HCID 1049PyridineHCID 61147Bromoacetyl bromideHCID 102651411-Methyl-5-(2-fluorobenzoyl)-1,2,3,4-tetrahydroquinoxaline

生成物 1

HCID 104755351-Methyl-4-bromoacetyl-5-(2-fluorobenzoyl)-1,2,3,4-tetrahydroquinoxaline

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 1-methyl-5-(2-fluorobenzoyl)-1,2,3,4-tetrahydroquinoxaline (11.99 g) and pyridine (4.04 g) in methylene chloride (200 ml) was dropwise added a solution of bromoacetyl bromide (5.09 ml) in methylene chloride (10 ml) under stirring at a temperature below 10° C. and the mixture was stirred for 3 hours at the same temperature. The reaction mixture was washed with water twice and dried. Removal of the solvent afforded viscous oil. The viscous oil was triturated with diisopropyl ether, collected by filtration, washed with diisopropyl ether and dried to give 1-methyl-4-bromoacetyl-5-(2-fluorobenzoyl)-1,2,3,4-tetrahydroquinoxaline (17.18 g).

後処理

  1. stirringthe mixture was stirred for 3 hours at the same temperature
  2. washThe reaction mixture was washed with water twice
  3. customdried
  4. customRemoval of the solvent
  5. customafforded viscous oil
  6. customThe viscous oil was triturated with diisopropyl ether
  7. filtrationcollected by filtration
  8. washwashed with diisopropyl ether
  9. customdried

出典と根拠

ORDレコード
ord-2d578288fbab40fdaa93168904260457
出典データセット
uspto-grants-1994_06
特許番号
US05322842

反応ノート

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