Methane → HCID 178519944, 화합물

HRID 356291

반응식

HRID 356291 반응식
C([O:5][CH2:6][CH3:7])(=O)CO.[NH2:8][C:9]1[C:14]([NH2:15])=[CH:13][N:12]=[CH:11][N:10]=1.C>>[OH:5][CH2:6][C:7]1[NH:8][C:9]2[N:10]=[CH:11][N:12]=[CH:13][C:14]=2[N:15]=1

참가 물질

4

반응물 3

HCID 297MethaneHCID 12184Ethyl GlycolateHCID 837034,5-Diaminopyrimidine

생성물 1

HCID 178519944HCID 178519944, 화합물수율 58.5%

반응 조건

온도
140 °C

실험 절차

8.58 g of ethyl glycolate were added to 2.27 g of 4,5-diaminopyrimidine, and the resulting mixture was stirred at 140° C. for 2 hours. At the end of this time, the reaction mixture was freed from ethyl glycolate by distillation under reduced pressure. The residue thus obtained was decolorized by activated charcoal and crystallized by trituration with ethanol, to give 1.81 g of the title compound having Rf=0.27 (on silica gel thin layer chromatography using a 10:1 by volume mixture of ethyl acetate and methanol as the developing solvent).

후처리

  1. distillationAt the end of this time, the reaction mixture was freed from ethyl glycolate by distillation under reduced pressure
  2. customThe residue thus obtained
  3. customcrystallized by trituration with ethanol

출처 및 근거

ORD 기록
ord-587a2a1899d046029fd55ec504cbd6b7
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834501

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