2,2,7,7-tetrabutyl-1,3,6,8,2,7-tetroxadistannecane synthesis

Yield:5271-60-3 96%

Reaction Conditions:

in toluene;Dean-Stark;Reflux;

Steps:

1,1,6,6-Tetra-nbutyl1,6distanna2,5,7,10tetraoxacyclodecane (1/2)

was prepared using dibutyltin oxide (4.05 g,0.0163 mol) and ethylene glycol (0.92 mL, 1.021, 0.0163 mol, 1.0equiv.). The reactants were taken in a three-neck flask containingdry toluene (100 mL) equipped with a Dean and Stark moisturetrap. The reaction mixture was stirred under reflux conditions(dibutyltin oxide dissolves) until a constant volume of 0.3 mL liquidhad collected in the trap.The flask containing the product (a clear yellow toluene solution)was gradually cooled to room temperature. The solutiondeposited white crystals which were isolated by filtration, washedwith toluene and dried under vacuum; yield 4.579 g (96%). Thesewere recrystallized from methylene chloride. The M.p. is 223-226.5 C (lit. 223-229). Exposure of the product to air, overnight,did not affect the M.p. Found: C, 41.36; H, 7.45; Sn, 40.45%; mol.wt. in CHCl3,650. C20H44O4Sn2 Cald.: C, 40.99; H, 7.57; Sn,40.52%; mol. wt. 586). The 119Sn NMR spectrum of initiator 1was recorded and the structure was confirmed.

References:

Mohite, Kavita K.;Garnaik, Baijayantimala [Polyhedron,2020,vol. 175,art. no. 114202]