تفاعل #565871

معادلة التفاعل

5-amino-7-methoxy-2,2-dimethylchromene

compound

3-Chloro-4-nitro-2-naphthalenecarboxylic Acid

potassium acetate

2-propanol

→

3-[(2,2-Dimethyl-7-methoxy-2H-chromen-5-yl)amino]-4-nitro-2-naphthalene-carboxylic Acid

المذيبات

triethylamine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution is refluxed for 5 days
2. 2
   أخرىis then evaporated under reduced pressure
3. 3
   workup.ADDITIONThe residue is taken up in a 1/1 mixture of dichloromethane and 1N aqueous HCl solution
4. 4
   استخلاصAfter extraction of the aqueous phase
5. 5
   workup.ADDITIONthe combined organic phases are treated in customary manner
6. 6
   أخرىto be isolated

الإجراء التجريبي

To 3.3 g of 5-amino-7-methoxy-2,2-dimethylchromene there are added 3 g of the compound obtained in Step 3 above, 3.4 g of potassium acetate, 375 mg of Cu(OAc)2.H2O and 120 ml of 2-propanol containing 3.8 ml of triethylamine. The solution is refluxed for 5 days and is then evaporated under reduced pressure. The residue is taken up in a 1/1 mixture of dichloromethane and 1N aqueous HCl solution. After extraction of the aqueous phase, the combined organic phases are treated in customary manner. Chromatography over silica gel (dichloromethane/methanol: gradient from 0.1 to 1%) allows the expected product to be isolated.

المصدر