Calcium Carbonate → HCID 18706700、化合物

HRID 1422222ノート

反応式

HRID 1422222 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH2:16]Br)[CH:3]=1.C(=O)([O-])[O-:19].[Ca+2]>O1CCOCC1.O>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[C:7]([O:14][CH3:15])[C:8]([O:12][CH3:13])=[N:9]2)=[C:4]([CH2:16][OH:19])[CH:3]=1

参加物

5

反応物 2

HCID 10112Calcium CarbonateHCID 23298010HCID 23298010、化合物

生成物 1

HCID 18706700HCID 18706700、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

11.5 g (31.85 mmol) of 7-bromo-5-bromomethyl-2,3-dimethoxy-quinoxaline are suspended at 20° C. in 100 ml of dioxane. 16.4 g (164 mmol) of calcium carbonate in 100 ml of water are then added and the mixture is heated at reflux for 24 hours. The dioxane is concentrated by evaporation and 300 ml of dichloromethane are added. The salt is filtered off, the organic phase is washed with brine and concentrated by evaporation and the residue is chromatographed on silica gel with ethyl acetate and hexane (1:1).

後処理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 24 hours
  3. concentrationThe dioxane is concentrated by evaporation and 300 ml of dichloromethane
  4. additionare added
  5. filtrationThe salt is filtered off
  6. washthe organic phase is washed with brine
  7. concentrationconcentrated by evaporation
  8. customthe residue is chromatographed on silica gel with ethyl acetate and hexane (1:1)

出典と根拠

ORDレコード
ord-e8cd4e97f26b4e49a8ca77d9eddbf969
出典データセット
uspto-grants-2000_06
特許番号
US06080743

反応ノート

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