反応 #53241

ord-d0a2792311094e53ba927cdb4a416d7a

反応方程式

N=C(N)N.O=C(O)O
guanidine carbonate
CCOC(=O)CC(C)=O
ethyl acetoacetate
Cc1cc(=O)nc(N)[nH]1
6-methyl-iso cytosine
収率 125.6%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction solution was gradually heated
  2. 2
    温度to reflux temperature
  3. 3
    その他Ethanol (300 mL) was evaporated
  4. 4
    温度the reaction mixture was heated
  5. 5
    温度under reflux for two hours
  6. 6
    温度After the reaction mixture was cooled
  7. 7
    workup.ADDITION300 mL of hexane was added
  8. 8
    ろ過The resulting precipitate was filtered
  9. 9
    洗浄washed
  10. 10
    その他dried

実験手順

Dry ethanol (600 mL), 91.89 g of guanidine carbonate, and 146.1 g of ethyl acetoacetate were added to a 1 L flask. The reaction solution was gradually heated to reflux temperature and stirred overnight. Ethanol (300 mL) was evaporated, and the reaction mixture was heated under reflux for two hours. After the reaction mixture was cooled, 300 mL of hexane was added. The resulting precipitate was filtered, washed and dried. 119.3 g of 6-methyl-iso cytosine was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06858359B2uspto-grants-2005_02