تفاعل #42187
ord-bdd7dcee9f5a4cce96a47a8ac1c2f344
المذيبات
ظروف التفاعل
المعالجة
- 1أخرىA 100-ml four-necked flask was equipped with a stirrer
- 2workup.ADDITIONadded into the flask
- 3أخرىThe flask was purged with argon
- 4workup.STIRRINGby stirring at 125° C. for 4 hours
- 5أخرىAfter the completion of the reaction, 45 ml of xylene and 50 ml of saturated sodium chloride solution
- 6workup.ADDITIONwere added
- 7أخرىfollowed by separation
- 8أخرىThe 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. 7.536 g (48 mmol) of bromobenzene, 6.769 g (40 mmol) of diphenylamine, 4.613 g (48 mmol) of sodium-tert-butoxide, 0.009 g (0.04 mmol) of palladium (II) acetate and 5 ml of xylene were weighed in the flask, followed by stirring. Further, 0.074 g (0.12 mmol) of 2-biphenylyl-di-tert-butylphosphonium tetraphenylborate obtained in Example B-10 was weighed in air and added into the flask. The flask was purged with argon, followed by stirring at 125° C. for 4 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 8.537 g of triphenylamine (yield: 87 mol % based on diphenylamine). The melting point was 125-126° C.