3-Methoxybenzene-1,2-diamine → 5-Methoxyquinoxaline

HRID 275788

반응식

HRID 275788 반응식
O.S(=O)(O)[O-].[Na+].[CH:7]([CH:9]=O)=O.[NH2:11][C:12]1[C:17]([NH2:18])=[CH:16][CH:15]=[CH:14][C:13]=1[O:19][CH3:20]>O.C(O)C.Cl>[CH3:20][O:19][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:12]=1[N:11]=[CH:7][CH:9]=[N:18]2

참가 물질

6

반응물 2

HCID 1842683-Methoxybenzene-1,2-diamineHCID 23685989Glyoxal-sodium bisulfite hydrate

생성물 1

HCID 132383925-Methoxyquinoxaline수율 77.9%

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

Glyoxal sodium bisulphite hydrate (10.0 g) in water (80 ml) was warmed to 60° C. then a solution of 2,3-diaminoanisole (3.40 g) in ethanol (40 ml) was added. The stirred mixture was then heated to 80° C. for 1 h before addition of concentrated hydrochloric acid (6 drops). Heating was continued for 1 h. It was allowed to cool overnight, concentrated in vacuo and poured into aqueous potassium carbonate (40 ml). Ethyl acetate (3×100 ml) extracts were washed with water (100 ml) and saturated brine (50 ml) then dried over anhydrous magnesium sulphate, filtered and evaporated in vacuo to afford the title compound as a yellow solid (3.07 g).

후처리

  1. temperatureHeating
  2. temperatureto cool overnight
  3. concentrationconcentrated in vacuo
  4. additionpoured into aqueous potassium carbonate (40 ml)
  5. washEthyl acetate (3×100 ml) extracts were washed with water (100 ml) and saturated brine (50 ml)
  6. dry with materialthen dried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-a693d42e681d4e4b8ec4f4f16a2ddd56
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06353010B1

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