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Sodium methanolate methanol → 2-Methoxypyrido[2,3-d]pyrimidin-7(8H)-one

HRID 385555
ノート
印刷プレビュー

反応式

HRID 385555 の反応式
[NH2:1][C:2]1[C:7](/[CH:8]=[CH:9]/[C:10](OCC)=[O:11])=[CH:6][N:5]=[C:4]([O:15][CH3:16])[N:3]=1.C[O-].[Na+].CO>CO>[CH3:16][O:15][C:4]1[N:5]=[CH:6][C:7]2[CH:8]=[CH:9][C:10](=[O:11])[NH:1][C:2]=2[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 23694274Sodium methanolate methanolHCID 68105238HCID 68105238、化合物

生成物 1

HCID 578153292-Methoxypyrido[2,3-d]pyrimidin-7(8H)-one収率 79.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 0.87 g of ethyl (2E)-3-(4-amino-2-methoxypyrimidin-5-yl)acrylate in 50 mL of methanol, 2.31 g of a 28% sodium methoxide/methanol solution was added at room temperature, and the mixture was heated under reflux while stirring for 4 hours. The reaction mixture was cooled to room temperature, and the solvent was then distilled off under reduced pressure. To the resultant residue, a saturated aqueous ammonium chloride solution and chloroform were added, the organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and the extract were combined, the resultant solution was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The solid thus obtained was washed with diethyl ether to obtain 0.55 g of 2-methoxypyrido(2,3-d)pyrimidin-7(8H)-one as a yellow solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. distillationthe solvent was then distilled off under reduced pressure
  4. additionTo the resultant residue, a saturated aqueous ammonium chloride solution and chloroform were added
  5. customthe organic layer was separated
  6. extractionthe aqueous layer was extracted with chloroform
  7. dry with materialthe resultant solution was dried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. customThe solid thus obtained
  10. washwas washed with diethyl ether

出典と根拠

ORDレコード
ord-bf848f12d5564931a95692bc58a65987
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367831B2

反応ノート

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