Dimethylformamide → Methyl 2-(4,6-dimethoxypyrimidin-2-yloxy)-6-methylnicotinate

HRID 1770076노트

반응식

HRID 1770076 반응식
[OH:1][C:2]1[N:11]=[C:10]([CH3:12])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C(=O)([O-])[O-].[K+].[K+].Cl[C:20]1[N:25]=[C:24]([O:26][CH3:27])[CH:23]=[C:22]([O:28][CH3:29])[N:21]=1.CN(C)C=O>O>[CH3:29][O:28][C:22]1[CH:23]=[C:24]([O:26][CH3:27])[N:25]=[C:20]([O:1][C:2]2[N:11]=[C:10]([CH3:12])[CH:9]=[CH:8][C:3]=2[C:4]([O:6][CH3:7])=[O:5])[N:21]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 51523232-Chloro-4,6-dimethoxypyrimidineHCID 178497913HCID 178497913, 화합물

생성물 1

HCID 20095253Methyl 2-(4,6-dimethoxypyrimidin-2-yloxy)-6-methylnicotinate수율 8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

5.0 g (0.03 mol) of methyl 2-hydroxy-6-methylnicotinate, 5.0 g (0.03 mol) of potassium carbonate, 5.7 g (0.03 mol) of 2-chloro-4,6-dimethoxypyrimidine and 50 ml of N,N-dimethylformamide were weighed, and were reacted at 100° C. for 4 hours. The reaction mixture was then poured into water, and was extracted with 100 ml of ethyl acetate. The organic layer was then washed with water and a saturated sodium chloride aqueous solution. After drying with anhydrous sodium sulfate, the solvent was distilled off, and the residue was purified by silica gel column chromatography to obtain 0.73 g of the aimed product.

후처리

  1. customwere reacted at 100° C. for 4 hours
  2. extractionwas extracted with 100 ml of ethyl acetate
  3. washThe organic layer was then washed with water
  4. dry with materialAfter drying with anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-9798b391204444be9315ebb2b3fecfb5
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05385880

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