Methyl iodide → 5-Methoxyquinoxaline

HRID 2374156

反応式

HRID 2374156 の反応式
[N:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([OH:11])[C:5]=2[N:4]=[CH:3][CH:2]=1.[C:12]([O-])([O-])=O.[K+].[K+].IC>CN(C=O)C>[CH3:12][O:11][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[N:4]=[CH:3][CH:2]=[N:1]2

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 1356902745-Quinoxalinol

生成物 1

HCID 132383925-Methoxyquinoxaline

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

To quinoxalin-5-ol (0.43 g) dissolved in DMF (6 ml) was added K2CO3 (2.5 eq.) and KI (0.2 eq.). To this mixture was then added dropwise iodomethane (1.2 eq.). The resulting mixture then heated to 50° C. overnight. The reaction mixture was subsequently partitioned between satd. NaHCO3 and EtOAc, the EtOAc layer backwashed with water and brine, dried over Na2SO4, and concentrated to dryness under vacuum. The crude material was then purified by SGC (MeOH:DCM) affording 5-methoxyquinoxaline. MS (ESI+) for m/z 160 [M+H]+.

後処理

  1. customThe reaction mixture was subsequently partitioned between satd
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated to dryness under vacuum
  4. customThe crude material was then purified by SGC (MeOH:DCM)

出典と根拠

ORDレコード
ord-c80d808245104e7db92fadefdc7f9a71
出典データセット
uspto-grants-2008_12
特許番号
US07462600B2

関連ノート

読み込み中…