反応 #64717

ord-6029f0ddbc5f49ef962aebcb76173fc8

反応方程式

O=C([O-])O
hydrogencarbonate
CO
methanol
COc1ccc(NC(=O)c2ccccc2C(c2ccc(OC(C)=O)cc2)c2ccc(OC(C)=O)cc2)c(OC)c1
Compound 2
COc1ccc(NC(=O)c2ccccc2C(c2ccc(OC(C)=O)cc2)c2ccc(OC(C)=O)cc2)c(OC)c1
2-[Bis(4-acetoxyphenyl)methyl]-N-(2,4-dimethoxyphenyl)benzamide
COc1ccc(NC(=O)c2ccccc2C(c2ccc(O)cc2)c2ccc(O)cc2)c(OC)c1
desired product
収率 56.0%
COc1ccc(NC(=O)c2ccccc2C(c2ccc(O)cc2)c2ccc(O)cc2)c(OC)c1
2-[Bis(4-hydroxyphenyl)methyl]-N-(2,4-dimethoxyphenyl)benzamide
収率 56.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the suspension was heated
  2. 2
    温度under reflux for 30 minutes
  3. 3
    濃縮The resulting mixture was concentrated under reduced pressure, and water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    抽出The resulting mixture was extracted with ethyl acetate
  6. 6
    乾燥the extract was dried over anhydrous magnesium sulfate
  7. 7
    濃縮After concentration under reduced pressure
  8. 8
    その他the residue was recrystallized

実験手順

In a mixture of 50 ml of saturated aqueous sodium. hydrogencarbonate solution and 50 ml of methanol was suspended 2.6 g of Compound 2 prepared in Example 1, and the suspension was heated under reflux for 30 minutes. The resulting mixture was concentrated under reduced pressure, and water was added to the residue. The resulting mixture was extracted with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate. After concentration under reduced pressure, the residue was recrystallized to afford 1.23 g of the desired product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05413997uspto-grants-1995_05