Methane → HCID 178519944、化合物

HRID 356291

反応式

HRID 356291 の反応式
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

参加物

4

反応物 3

HCID 297MethaneHCID 12184Ethyl GlycolateHCID 837034,5-Diaminopyrimidine

生成物 1

HCID 178519944HCID 178519944、化合物収率 58.5%

反応条件

温度
140 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-587a2a1899d046029fd55ec504cbd6b7
出典データセット
uspto-grants-1998_11
特許番号
US05834501

関連ノート

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