تفاعل #816318

معادلة التفاعل

dodecene

3-benzyloxycarbonylaminopropylphosphonous acid

→

3-benzyloxycarbonylaminopropyl(dodecyl)phosphinic acid

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONcontaining 0.6 g
2. 2
   workup.ADDITIONof t-butylcyclohexylperdicarbonate is added within 15 minutes
3. 3
   workup.STIRRINGstirring at 80°
4. 4
   workup.WAITis continued for 2 hours
5. 5
   أخرىthe solvent is removed by means of a rotary evaporator
6. 6
   أخرىThe residue is triturated with petroleum ether (60°-80°)
7. 7
   ترشيحfiltered
8. 8
   أخرىdried

الإجراء التجريبي

A solution of 1.30 g of dodecene in 6 ml of dry toluene is heated to 80° under an atmosphere of argon. To this solution a suspension of 2.0 g of 3-benzyloxycarbonylaminopropylphosphonous acid in 30 ml of dry tolpene containing 0.6 g of t-butylcyclohexylperdicarbonate is added within 15 minutes. The reaction mixture is then stirred at 80° for 2 hours. An additional amount of 0.6 g of the radical initiator is added and stirring at 80° is continued for 2 hours. Then, the reaction mixture is cooled to room temperature and the solvent is removed by means of a rotary evaporator. The residue is triturated with petroleum ether (60°-80°), filtered and dried to give 3-benzyloxycarbonylaminopropyl(dodecyl)phosphinic acid as a white solid, m.p. 115°-6°; 31P-NMR: δ=+58.7 ppm (CDCl3).

المصدر