Ethanol → 2-Amino-6-methylpyrimidin-4-one

HRID 1071788

反応式

HRID 1071788 の反応式
C(O)C.C(=O)(O)O.[NH2:8][C:9]([NH2:11])=[NH:10].[C:12](OCC)(=[O:17])[CH2:13][C:14]([CH3:16])=O>O>[NH2:10][C:9]1[NH:11][C:12](=[O:17])[CH:13]=[C:14]([CH3:16])[N:8]=1

参加物

5

反応物 3

HCID 702EthanolHCID 8868Ethyl AcetoacetateHCID 286947Carbonic acid-guanidine (1:1)

生成物 1

HCID 1354020552-Amino-6-methylpyrimidin-4-one収率 68%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The title compound was prepared according to a literature method (Hirschberg, J. H. K., Beijer, F. H., van Aert, H. A., Magusin, P. C. M., Sijbesma, R. P., Meijer, E. W., Macromolecules, 1999, 32, 2696-2705, the disclosure of which is totally incorporated herein by reference). To a 1 liter round bottom flask under an inert argon atmosphere was added 650 milliliters of dry ethanol and 90.08 grams (0.5 mole) of guanidine carbonate. Thereafter, with good stirring was added dropwise over 2 hours 130.17 grams (1 mole) of ethyl acetoacetate, after which heat was applied and the mixture refluxed for 15 hours. The mixture was then cooled to room temperature and 800 milliliters of deionized water was slowly added to induce precipitation of the product. Subsequent vacuum filtration and washing with cold acetone secured the anticipated product in 68 percent yield (mp 311° C.). All physical properties were in accord with the reported properties.

後処理

  1. temperatureafter which heat
  2. temperaturethe mixture refluxed for 15 hours
  3. customprecipitation of the product
  4. filtrationSubsequent vacuum filtration
  5. washwashing with cold acetone

出典と根拠

ORDレコード
ord-07d20abc724944eb948658e4ce1f88b7
出典データセット
uspto-grants-2005_06
特許番号
US06906118B2

関連ノート

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