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Methanol → 4,6-Dimethoxy-2-methylpyrimidin-5-amine

HRID 1628507
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HRID 1628507 반응식
[CH3:1][O-:2].[Na+].Cl[C:5]1[C:10]([NH2:11])=[C:9](Cl)[N:8]=[C:7]([CH3:13])[N:6]=1.[CH3:14][OH:15]>>[CH3:1][O:2][C:5]1[C:10]([NH2:11])=[C:9]([O:15][CH3:14])[N:8]=[C:7]([CH3:13])[N:6]=1
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참가 물질

4

반응물 3

HCID 887MethanolHCID 7366744,6-Dichloro-2-methylpyrimidin-5-amineHCID 10942334Sodium Methoxide

생성물 1

HCID 212392004,6-Dimethoxy-2-methylpyrimidin-5-amine수율 100%

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온도
70 °C

실험 절차

Sodium methoxide (28% solution in methanol, 150 mL) was added dropwise to a stirred solution of 4,6-dichloro-2-methylpyrimidin-5-amine (15.0 g, 84.3 mmol) in methanol (150 mL) at 0° C., and the mixture was stirred at room temperature for 1 hr, at 70° C. for 6 hr. The mixture was concentrated, diluted with aqueous saturated ammonium chloride and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give the title compound as a yellow solid (14.2 g, 84.3 mmol, 100%).

후처리

  1. concentrationThe mixture was concentrated
  2. additiondiluted with aqueous saturated ammonium chloride
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-63a004bd402445b68b0cddc25f7818f6
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785460B2

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