SYNTHESIS OF ANTIMONY(V) OCTAETHYLPORPHYRINS THAT CONTAIN A SIGMA-BONDED ELEMENT CARBON BOND

被引：25

作者：

AKIBA, KY ^{[1
]}

ONZUKA, Y ^{[1
]}

ITAGAKI, M ^{[1
]}

HIROTA, H ^{[1
]}

YAMAMOTO, Y ^{[1
]}

机构：

[1] UNIV TOKYO,FAC SCI,BUNKYO KU,TOKYO 113,JAPAN

来源：

ORGANOMETALLICS | 1994年 / 13卷 / 07期

关键词：

D O I：

10.1021/om00019a041

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Antimony(V) octaethylporphyrins with sigma-bonded antimony-carbon bonds were synthesized: [(OEP)SbR(OH)]+PF6- (1a-PF6, R = Me; 1b-PF6, R = Et) and [(OEP)SbMe2]+PF6- (2a-PF6). Compounds la and lb were prepared by the reaction of [(OEP)Sb(OMe)(OH)]+Cl- (6) with an excess amount of R3Al, and 2a was obtained from (OEP)SbCl (3) and an excess amount of Me3Al. The compounds 1a-PF6, 1b-PF6, and 2a-PF6 were remarkably stable toward air and moisture in comparison with corresponding group 13 and 14 analogues. The H-1 NMR of these compounds showed characteristic axial alkyl signals at very high field (delta -6.10 in 1a-PF6, -5.87 and -4.33 in 1b-PF6, and -6.73 in 2a-PF6) because of the ring current effect of the porphyrin nucleus. X-ray crystallographic analysis of 2a-PF6 is Presented; space group P2(1)/m, a = 11.777-(3) angstrom, b = 18.183(4) angstrom, c = 9.712(2) angstrom, beta = 100.75(2)degrees, R = 0.051.

引用

页码：2800 / 2803

页数：4

共 28 条

[11] NEW MONTE-CARLO METHOD FOR PHASE DETERMINATION [J].