N,N'-Dimethylurea → 6-(3-pyridyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione

HRID 65145

反応式

HRID 65145 の反応式
[C:1]([CH2:9][C:10]([O:12]CC)=O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.[CH3:15][NH:16][C:17]([NH:19][CH3:20])=[O:18].C(=O)(O)[O-].[Na+]>Cl.C(O)C>[N:4]1[CH:5]=[CH:6][CH:7]=[C:2]([C:1]2[N:19]([CH3:20])[C:17](=[O:18])[N:16]([CH3:15])[C:10](=[O:12])[CH:9]=2)[CH:3]=1

参加物

6

反応物 3

HCID 7293N,N'-DimethylureaHCID 222197Ethyl 3-oxo-3-(pyridin-3-yl)propanoateHCID 516892Sodium Bicarbonate

生成物 1

HCID 140964686-(3-pyridyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione収率 35.2%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 702Ethanol溶媒

実験手順

To a mixture of ethyl nicotinoylacetate (2.30 g) and N,N'-dimethylurea (1.05 g) were added conc. hydrochloric acid (a few drops) and ethanol (1 ml) and the mixture was stirred at 110°-115° C. for 4 hours under reduced pressure (30 mmHg). After being cooled to ambient temperature, the solution was adjusted to pH 7.0 with an aqueous solution of sodium bicarbonate and extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate and evaporated to give 6-(3-pyridyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione (0.91 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-f9b5bfc73ccf429d972dda2f5938f576
出典データセット
uspto-grants-1986_09
特許番号
US04612376

関連ノート

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