乙酰乙酸乙酯 → HCID 178488949，化合物

HRID 1082082

反应方程式

HRID 1082082 反应方程式
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

参与物

5

反应物 3

HCID 8868乙酰乙酸乙酯HCID 11430碳酸钾HCID 123262194-甲氧基苯甲脒盐酸盐

产物 1

HCID 178488949HCID 178488949，化合物

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-23fbbe22de624dc692ed81c6ea82baf6
来源数据集
uspto-grants-1996_12
专利号
US05589477

关联笔记

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