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

HRID 2082727

反応式

HRID 2082727 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;l -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. temperaturewas heated
  2. temperatureunder reflux
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-d52d8857df584e0b95928f02124bd8e0
出典データセット
uspto-grants-1978_04
特許番号
US04082751

関連ノート

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