2-Amino-4,6-dimethyl pyrimidine → Methyl 3-[[(4,6-dimethylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl]-2-thiophenecarboxylate

HRID 256264

반응식

HRID 256264 반응식
[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[CH3:10][O:11][C:12]([C:14]1[S:15][CH:16]=[CH:17][C:18]=1[S:19]([N:22]=[C:23]=[O:24])(=[O:21])=[O:20])=[O:13]>C(#N)C>[CH3:9][C:4]1[CH:5]=[C:6]([CH3:8])[N:7]=[C:2]([NH:1][C:23]([NH:22][S:19]([C:18]2[CH:17]=[CH:16][S:15][C:14]=2[C:12]([O:11][CH3:10])=[O:13])(=[O:20])=[O:21])=[O:24])[N:3]=1

참가 물질

4

반응물 2

HCID 130212-Amino-4,6-dimethyl pyrimidineHCID 1572962-Thiophenecarboxylic acid, 3-(isocyanatosulfonyl)-, methyl ester

생성물 1

HCID 13390185Methyl 3-[[(4,6-dimethylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl]-2-thiophenecarboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To 1.23 g of 2-amino-4,6-dimethyl pyrimidine in 30 ml of anhydrous acetonitrile was added with stirring 2.7 g of 2-methoxycarbonyl-3-thiophenesulfonylisocyanate. The mixture was heated to the boiling point, whereupon all of the insoluble material dissolved and the mixture was allowed to cool. After stirring for two hours the mixture was filtered to remove the desired product which had precipitated as a white solid. After washing with anhydrous ethyl ether the product melted at 191°-193° with decomposition and showed absorption peaks by nuclear magnetic resonance at 3.8 ppm for the methoxy group, 2.44 ppm for the two methyl groups on the pyrimidine ring, a peak at 7.0 consistent for the hydrogen in the pyrimidine ring and a peak at 7.42 for the hydrogens on the thiophene ring. The infrared absorption spectrum showed absorption peaks at 1720 and 1700 cm-1 consistent for the two carbonyl groups present in the desired product.

후처리

  1. temperatureThe mixture was heated to the boiling point
  2. dissolutionwhereupon all of the insoluble material dissolved
  3. temperatureto cool
  4. filtrationwas filtered
  5. customto remove the desired product which
  6. customhad precipitated as a white solid
  7. washAfter washing with anhydrous ethyl ether the product melted at 191°-193° with decomposition
  8. customabsorption peaks by nuclear magnetic resonance at 3.8 ppm for the methoxy group, 2.44 ppm for the two methyl groups on the pyrimidine ring
  9. customThe infrared absorption spectrum
  10. customabsorption peaks at 1720 and 1700 cm-1 consistent for the two carbonyl groups

출처 및 근거

ORD 기록
ord-6e97632cdbeb48bd8b52b2a6d32ce0b8
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04701535

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