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

HRID 437432

반응식

HRID 437432 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록
ord-7026d10e25c44287b5b29e96cc6ed433
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04031093

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