Réaction #93836

Équation de réaction

water

bis(tributyltin) oxide

N,N-dibutylethanolamine

→

N,N-Dibutylaminoethyl Tributylstannyl Ether

Solvants

benzene

Conditions de réaction

Traitement

1. 1
   Températureheated
2. 2
   Températureto reflux in a system that
3. 3
   Autreto collect in the Dean-Starke tube
4. 4
   Températureafter refluxing for a period of 22 hours a total of 1.8 ml of water (theory 1.8 ml)
5. 5
   Autrehad collected
6. 6
   AutreA rotating evaporator
7. 7
   Autreto remove the benzene

Mode opératoire

N,N-Dibutylaminoethyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 34.6 gm (0.2 mole) N,N-dibutylethanolamine in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After 30 minutes water began to collect in the Dean-Starke tube and after refluxing for a period of 22 hours a total of 1.8 ml of water (theory 1.8 ml) had collected. A rotating evaporator is used to remove the benzene and to provide 95.1 gm of red-orange liquid. This is fractionated at reduced pressure with collection at 163°-166° C. at 0.7 mm of 73.1 gm of yellow liquid (Percent yield - 79). Infrared spectral analysis shows this to be the desired ether.

Source