William Quintana

The first half-sandwich d0-metallacarboranes stabilized by metal–nitrogen sigma bond using C(cage)-appended anionic alkylamido moiety: a synthetic investigation

Abstract The 1:1 molar reaction of the potassium/dilithium triple salt of the [ nido -7-(NHCH 2 )-7,8-C 2 B 9 H 10 ] 3− trianion with anhydrous MCl 4 in dry tetrahydrofuran (THF) at −78°C, followed by extraction with dry benzene and precipitation with n -pentane, resulted in the formation of the corresponding novel half-sandwich d 0 -metallacarborane, closo -1-M[(Cl)(THF) n ]-2-(1-σ-NHCH 2 )-2,3-η 5 -C 2 B 9 H 10 [M=Zr ( 3 ), n =1; Ti ( 4 ), n =0] in 57% and 49% yields, respectively.

Synthesis and characterization of a protected amino alcohol containing ortho-carborane

Abstract The reaction between the alkyne, N- (5-Benzyloxy-2-pentynyl) phthalimide and decaborane (14) in the presence of dimethyl sulfide resulted in the isolation of 1-C6H4 (CO) 2NCH2-2-C6H5CH2OCH2CH2-1, 2-C2B10H10 (5) , 1-methylphthalimido-2-ethylbenzyl ether-o-carborane, in moderate yield. Compound 5 was characterized by single crystal X-ray diffraction study. Compound 5 crystallizes in the P 1 space group, a=10.5328 (5) A, b=11.9209 (6) A, c=10.3451 (3) A, α=110.492 (3) °, β=102.868 (3) °, γ=87.279 (2) °, Z=2, Dcalc=1.226 g\cm3, R=0.0491 for 3521 reflections with F>4.0σ. Deprotection of the ether linkage of 5 results in the formation of 1-C6H4 (CO) 2NCH2-2-HOCH2CH2-1, 2-C2B10H10 (6) , 1-methylphthalimido-2-ethylalcohol-o-carborane. The transformation is accomplished by hydrogenation of (5) over a Pd\C catalyst and resulted in the efficient conversion of (5) into (6) (83% yield) . Experimental details and analytical data leading to the identification of the reported compounds is provided.