تفاعل #1114495

معادلة التفاعل

1-bromopyrene

2-naphthaleneboronic acid

tripotassium phosphate

dimethylformamide

→

1-(2-naphthyl)pyrene

المردود 91.7%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling the solution to room temperature
2. 2
   workup.STIRRINGby stirring at room temperature for 0.5 hours
3. 3
   ترشيحThe precipitated solid was collected by filtration
4. 4
   غسيلwashed twice with 100 ml of water
5. 5
   workup.DISSOLUTIONThe resultant solid was dissolved in 200 ml of dichloromethane
6. 6
   تجفيفdried over magnesium sulfate
7. 7
   أخرىevaporated
8. 8
   ترشيحfiltered
9. 9
   أخرىThe filtrate was evaporated
10. 10
    غسيلthe residue was washed twice with 100 ml of methanol
11. 11
    ترشيحthe precipitated solid was collected by filtration
12. 12
    أخرىThe solid was vacuum-dried

الإجراء التجريبي

A mixed solution of 7.0 g of 1-bromopyrene, 4.7 g of 2-naphthaleneboronic acid, 11.6 g of tripotassium phosphate, 1.8 g of tetrabutylammonium bromide, 0.11 g of palladium acetate and 248 ml of dimethylformamide was heated with stirring under a nitrogen gas flow at 130° C. for 5 hours. After cooling the solution to room temperature, 300 ml of water was injected, followed by stirring at room temperature for 0.5 hours. The precipitated solid was collected by filtration and then washed twice with 100 ml of water. The resultant solid was dissolved in 200 ml of dichloromethane, dried over magnesium sulfate, evaporated and then filtered using Celite. The filtrate was evaporated and the residue was washed twice with 100 ml of methanol, and then the precipitated solid was collected by filtration. The solid was vacuum-dried to obtain 7.5 g of 1-(2-naphthyl)pyrene.

المصدر