تفاعل #42164

معادلة التفاعل

chlorobenzene

diphenylamine

sodium-tert-butoxide

→

triphenylamine

المردود 91.8%

المذيبات

xylene

ظروف التفاعل

المعالجة

1. 1
   أخرىA 100-ml four-necked flask was equipped with a stirrer
2. 2
   workup.ADDITIONadded into the flask
3. 3
   أخرىThe flask was purged with argon
4. 4
   workup.STIRRINGby stirring at 100-120° C. for 10 hours
5. 5
   أخرىAfter the completion of the reaction, 45 ml of xylene and 50 ml of saturated sodium chloride solution
6. 6
   workup.ADDITIONwere added
7. 7
   أخرىfollowed by separation
8. 8
   أخرىThe organic phase was purified by column chromatography

الإجراء التجريبي

A 100-ml four-necked flask was equipped with a stirrer, a thermometer and a reflux condenser. 5.403 g (48 mmol) of chlorobenzene, 6.769 g (40 mmol) of diphenylamine, 4.613 g (48 mmol) of sodium-tert-butoxide, 0.002 g (0.01 mmol) of palladium (II) acetate and 5 ml of xylene were weighed in the flask, followed by stirring. Further, 0.021 g (0.04 mmol) of tri-tert-butylphosphonium tetraphenylborate obtained in Example A-1 was weighed in air and added into the flask. The flask was purged with argon, followed by stirring at 100-120° C. for 10 hours. After the completion of the reaction, 45 ml of xylene and 50 ml of saturated sodium chloride solution were added, followed by separation. The organic phase was purified by column chromatography to afford 9.008 g of triphenylamine (yield: 92 mol % based on diphenylamine). The melting point was 125-126° C.

المصدر