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

HRID 275788ノート

反応式

HRID 275788 の反応式
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

参加物

6

反応物 2

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

生成物 1

HCID 132383925-Methoxyquinoxaline収率 77.9%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a693d42e681d4e4b8ec4f4f16a2ddd56
出典データセット
uspto-grants-2002_03
特許番号
US06353010B1

反応ノート

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