Calcium Carbonate → HCID 18706700, 화합물

HRID 1422222노트

반응식

HRID 1422222 반응식
[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

참가 물질

5

반응물 2

HCID 10112Calcium CarbonateHCID 23298010HCID 23298010, 화합물

생성물 1

HCID 18706700HCID 18706700, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e8cd4e97f26b4e49a8ca77d9eddbf969
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080743

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