Methyl iodide → 5-Methoxyquinoxaline

HRID 2374156

반응식

HRID 2374156 반응식
[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

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 1356902745-Quinoxalinol

생성물 1

HCID 132383925-Methoxyquinoxaline

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

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]+.

후처리

  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)

출처 및 근거

ORD 기록
ord-c80d808245104e7db92fadefdc7f9a71
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07462600B2

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