TrisilanolPhenyl POSS synthesis

Yield:444315-26-8 87%

Reaction Conditions:

with lithium hydroxide monohydrate in methanol;water;acetone; for 18 h;Reflux;Solvent;

Steps:

(C6H5)7Si7O9(OH)3

The systhesis of phenyl-T7 was similar to the above two ways; however, the productwas directly distilled from the reaction mixture before neutralization. Thisintermediate (phenyl lithium salt) was filtered and washed with acetone, dried at80 C, then dissolved in trichloromethane, neutralized with aqueous HCl solution,and finally dried in the air atmosphere. The white solid was obtained in 87% yield.1H NMR (600 MHz, CDCl3-d6, d): 7.87-6.62 (Ph); 13C{1H} NMR (150 MHz,CDCl3, d): 134.38, 130.49, 127.62 (Ph); 29Si{1H} NMR (99 MHz, CDCl3, d):- 69.05, - 77.55 and - 78.52; FTIR (cm-1): 3416-3130 (-OH), 3093-3003 (C-H), 1590, 1426 (Ph), 1082 (Si-O-Si); MALDI-TOF-MS (m/z): 953.1 ([M ?Na?],calcd: 954.34).

References:

Ye, Miaofen;Wu, Yiwei;Zhang, Wenchao;Yang, Rongjie [Research on Chemical Intermediates,2018,vol. 44,# 7,p. 4277 - 4294]