Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl ester → Ethyl-2-methylthio-4-methyl-5-pyrimidine carboxylate

HRID 917393

반응식

HRID 917393 반응식
[C:1]([C:4](=[CH:10]OCC)[C:5]([O:7][CH2:8][CH3:9])=[O:6])(=O)[CH3:2].C[NH:15][C:16](=[NH:18])[SH:17].S(=O)(=O)(O)O.[C:24]([O-])(=O)C.[Na+]>CN(C)C=O>[CH3:2][C:1]1[C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])=[CH:10][N:18]=[C:16]([S:17][CH3:24])[N:15]=1

참가 물질

5

반응물 3

HCID 97734Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl esterHCID 517045Sodium AcetateHCID 178485225HCID 178485225, 화합물

생성물 1

HCID 188208Ethyl-2-methylthio-4-methyl-5-pyrimidine carboxylate수율 175.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

To 100 ml of N,N-dimethylformamide, 18.6 g (100 mmol) of ethyl 2-acetyl-3-ethoxyacrylate, 13.9 g (50 mmol) of sulfuric acid methylisothiourea and 8.2 g (100 mmol) of sodium acetate were suspended, followed by stirring at 80° C. for 4 hours. The reaction liquid was cooled and then poured in ice water. The crystal precipitated was filtered, washed with water and dried to obtain 18.6 g (yield: 88%) of ethyl 4-methyl-2-(methylthio)pyrimidine-5-carboxylate.

후처리

  1. customThe reaction liquid
  2. temperaturewas cooled
  3. customThe crystal precipitated
  4. filtrationwas filtered
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-5a9ad7cda0e547e5b20173e70c707922
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07273878B2

연결된 노트

불러오는 중…