تفاعل #64717

ord-6029f0ddbc5f49ef962aebcb76173fc8

معادلة التفاعل

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
المردود 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
المردود 56.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe suspension was heated
  2. 2
    درجة الحرارةunder reflux for 30 minutes
  3. 3
    تركيزThe resulting mixture was concentrated under reduced pressure, and water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    استخلاصThe resulting mixture was extracted with ethyl acetate
  6. 6
    تجفيفthe extract was dried over anhydrous magnesium sulfate
  7. 7
    تركيزAfter concentration under reduced pressure
  8. 8
    أخرىthe residue was recrystallized

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05413997uspto-grants-1995_05