Ethyl Acetoacetate → HCID 178429414、化合物

HRID 24963

反応式

HRID 24963 の反応式
C(=O)(O)O.[NH2:5][C:6]([NH2:8])=[NH:7].[C:9](OCC)(=[O:14])[CH2:10][C:11]([CH3:13])=O>C(O)C>[CH3:13][C:11]1[NH:5][C:6]([NH2:8])=[N:7][C:9](=[O:14])[CH:10]=1

参加物

4

反応物 2

HCID 8868Ethyl AcetoacetateHCID 286947Carbonic acid-guanidine (1:1)

生成物 1

HCID 178429414HCID 178429414、化合物収率 125.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

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.

後処理

  1. temperatureThe reaction solution was gradually heated
  2. temperatureto reflux temperature
  3. customEthanol (300 mL) was evaporated
  4. temperaturethe reaction mixture was heated
  5. temperatureunder reflux for two hours
  6. temperatureAfter the reaction mixture was cooled
  7. addition300 mL of hexane was added
  8. filtrationThe resulting precipitate was filtered
  9. washwashed
  10. customdried

出典と根拠

ORDレコード
ord-d0a2792311094e53ba927cdb4a416d7a
出典データセット
uspto-grants-2005_02
特許番号
US06858359B2

関連ノート

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