Synthesis of triphenylphosphonium trichlorogermanate and analogs. Preparation of germylenes from triphenylphosphonium trichlorogermanate

Abstract

ABSTRACT

Metal-Dependent Reactions of Bulky Metal(II) Amides M[N(SiMe3)2]2 with 3,3′-Disubstituted Binaphthols (HO)2C20H10(SiR3)2-3,3′: Selective Conversion of One Equivalent −OH Group to a Silyl Ether −OSiMe3

“…All manipulations were carried out using standard glovebox, Schlenk line, and syringe techniques . The compounds ( R )- 1 , ( R , R )- 8 , ( R )- 9 , ( S )- 9 , Be[N(SiMe 3 ) 2 ] 2 , Mg[N(SiMe 3 ) 2 ] 2 ·2THF, , Ca[N(SiMe 3 ) 2 ] 2 ·2THF, Zn[N(SiMe 3 ) 2 ] 2 , Ge[N(SiMe 3 ) 2 ] 2 , , and Sn[N(SiMe 3 ) 2 ] 2 were prepared according to literature procedures or slight variations thereof. 1 H, 13 C, and 9 Be NMR spectra were recorded using a Varian Inova spectrometer operating at 400, 100.6, or 56.2 MHz (respectively).…”

Synthesis of annulated furanoses by free-radical cyclization of haloalkenes derived from diacetone glucose

“…(7S)-10: oil; [a]25D +25.2°( c 2.4,CHC13); IR (film) 3600-3300 cm'1; NMR (300 MHz, CDC13) 7.30-7.27 (5H, aromatic), 5.76 (d,Jl2 = 3.6 Hz, 1 H, HI), 4.62 (s, -OCH20), 4.52 (t, =/12 = J23 = 3.6 Hz, I , H2), 4.30 (m, 1 , H5), 3.65 (dd, J4,3 = 1Í.0 Hz, «/4|5 = 2.4 Hz, 1 , H4), 3.30 (tt, </7|8m = e/7|8al = 11.8 Hz, t/7i8eq = é/7i8eq = 4.3 Hz, 1 , H7), 2.15-1.95 (m, 4 , H3, H6(eq), H8(eq), OH), 1. 40-1.25 (m, 2 H, H6(ax), H8(ax)), 1.44 (s, 3 H, CH3), 1.26 (s, 3 H, CH3)\ MS m/z 320 (M+ -15,3). Anal.…”

“…A procedure similar to those described by McGee and Confalone5f starting from 11 and using Se02 in diglyme at 200 °C for 30 min was followed. However, a 60% yield of alcohol 20 (and 25% recovery of 11) was obtained instead of the corresponding selenic ester.6f Mp and and 13C NMR spectra of alcohol 20 are identical with those of that derived from Se02-AcOH oxidation or LDA-HMPA-MoOPH hydroxylation: mp 212-214 °C; IR (CH2C12) 3400,1710; NMR 8.03 (dd, J = 8,1 Hz, 1 H, C-4 H), 7.48 (t, J = 8 Hz, 1 H, C-3 ), 7.1 (s, 1 H, C-ll H), 6.98 (dd, J = 8,1 Hz, 1 H, C-2 ), 5.09 (hr s, 1 H, CHO), 3.99 (s, 3 H, OMe), 3.97 (s, 3 H, OMe), 2.96 (dd, J = 18, 3 Hz, 1 H), 2.2 (hr d, J = 13 Hz, 1 ), 2.06 (m, 1 ), 1.9 (m, 1 ), 1.2 (m, 3 ), 1.06 (t, J = 7 Hz, 3 H, Me); 13C NMR 162 (s, CO), 156.78 (s), 153.7 (s), 145.76 (s), 139.8 (s), 137.7 (s) , 127.67 (d), 125.1 (s), 121.9 (s), 118.14 (s), 114.67 (d), 109.01 (d), 99.49 (d),63.84 (d,CO), 56.96 (q, OMe), 56.58 (q, OMe), 36.99 (t) , 30.62 (d), 29.17 (t), 28.91 (t), 11.23 (q); FAB MS m/e 355,354 (M+), 353, 246,185,154,137, 93. Anal. Caled for C21H2205: C, 71.17; H, 6.26.…”

Synthesis, structures and reactivity of novel germanium(ii) aryloxide and arylsulfide complexes

“…The bisamide Ge[N(SiMe 3 ) 2 ] 2 was purchased from Gelest, Inc. or synthesized via literature methods. [48][49][50] The compounds 2,6-diphenylphenol, 51 2,3,5,6-tetraphenylphenol 52 and 2,4,6-triisopropylbenzenethiol 53 were prepared according to literature methods, while 2,4,6-trimethylphenol, 2,6-diisopropylphenol, and iodomethane were purchased from Aldrich and used without further purification. Benzil was purchased from Aldrich and heated in vacuo at 100 ЊC for 12 h to remove water.…”