Ethyl Acetoacetate → HCID 178488949、化合物

HRID 1082082

反応式

HRID 1082082 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([NH2:10])=[NH:9])=[CH:6][CH:5]=1.[C:13](OCC)(=[O:18])[CH2:14][C:15]([CH3:17])=O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH:18][C:13]1[CH:14]=[C:15]([CH3:17])[N:10]=[C:8]([C:7]2[CH:11]=[CH:12][C:4]([O:3][CH3:2])=[CH:5][CH:6]=2)[N:9]=1

参加物

5

反応物 3

HCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 123262194-Methoxybenzamidine Hydrochloride

生成物 1

HCID 178488949HCID 178488949、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To the mixture of 10 g of 4-methoxybenzamidine hydrochloride, 7.7 g of ethyl acetoacetate and 16.3 g of potassium carbonate were added 120 ml of ethanol, and the mixture was heat-refluxed with stirring for 7 hours. The reaction mixture was cooled and filtered to remove insoluble substances. The filtrate was evaporated. Water was added to the residue to dissolve and then the resulting solution was neutralized with acetic acid. The precipitated crystals were filtered off, washed with water and dried. Whereby 10.9 g of the desired substance was obtained as white crystals. Melting point is 202° to 203° C.

後処理

  1. temperaturethe mixture was heat-refluxed
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. customto remove insoluble substances
  5. customThe filtrate was evaporated
  6. additionWater was added to the residue
  7. dissolutionto dissolve
  8. filtrationThe precipitated crystals were filtered off
  9. washwashed with water
  10. customdried
  11. customWhereby 10.9 g of the desired substance was obtained as white crystals

出典と根拠

ORDレコード
ord-23fbbe22de624dc692ed81c6ea82baf6
出典データセット
uspto-grants-1996_12
特許番号
US05589477

関連ノート

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