반응 #53241

ord-d0a2792311094e53ba927cdb4a416d7a

반응 방정식

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
수율 125.6%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction solution was gradually heated
  2. 2
    온도to reflux temperature
  3. 3
    기타Ethanol (300 mL) was evaporated
  4. 4
    온도the reaction mixture was heated
  5. 5
    온도under reflux for two hours
  6. 6
    온도After the reaction mixture was cooled
  7. 7
    workup.ADDITION300 mL of hexane was added
  8. 8
    여과The resulting precipitate was filtered
  9. 9
    세척washed
  10. 10
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06858359B2uspto-grants-2005_02