Acetic Acid → Ethyl 1,6-dihydro-6-oxo-2-(2-propoxyphenyl)pyrimidine-5-carboxylate

HRID 437432

反応式

HRID 437432 の反応式
COS(O)(=O)=O.[CH2:7]([O:10][C:11]1[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([NH2:15])=[NH:14])[CH2:8][CH3:9].C(=O)([O-])[O-].[K+].[K+].C([O:28][CH:29]=[C:30]([C:36](OCC)=O)[C:31]([O:33][CH2:34][CH3:35])=[O:32])C.C(O)(=O)C>C(O)C>[O:28]=[C:29]1[NH:15][C:13]([C:12]2[CH:16]=[CH:17][CH:18]=[CH:19][C:11]=2[O:10][CH2:7][CH2:8][CH3:9])=[N:14][CH:36]=[C:30]1[C:31]([O:33][CH2:34][CH3:35])=[O:32]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 6871Diethyl (ethoxymethylene)malonateHCID 11430Potassium CarbonateHCID 86734867n-Propoxybenzamidine methyl sulfate

生成物 1

HCID 12535801Ethyl 1,6-dihydro-6-oxo-2-(2-propoxyphenyl)pyrimidine-5-carboxylate収率 89%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-n-propoxybenzamidine methyl sulfate 7.4 g., 0.0255 mole), potassium carbonate (3.53 g., 0.025 mole), and diethyl ethoxymethylenemalonate (5.99 g., 0.0277 mole) in ethanol (80 ml.) was heated under reflux with stirring for 17 hours. The cooled mixture was added to ice-water (160 ml.) which was then acidified with glacial acetic acid. The precipitate was collected by filtration, washed with water, and dried to give the title compound (6.55 g., 89%), m.p. 106°-107°.

後処理

  1. temperatureunder reflux
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-7026d10e25c44287b5b29e96cc6ed433
出典データセット
uspto-grants-1977_06
特許番号
US04031093

関連ノート

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