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

HRID 1109721노트

반응식

HRID 1109721 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2d578288fbab40fdaa93168904260457
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05322842

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