heated under reflux for lOmin, then stirred for 24 h. The
product, a grey-white precipitate, was filtered off and dried in
uacuo. Yield: 90% (8.54 8). Anal. calc.: C, 42.0; H, 8.8%. Found:
C, 37.3; H, 8.0%. Mass loss in TG for decomposition to MgO:
calc.: 64.7%; found: 62.9%. IR (KBr) v/cm-l:2964, 2858 (s,
C-H str.); 1443, 1385, 1318 (m, C-H def.); 1129, 1100, 1068
(vs, C - 0 str.); 884 (m, C-C str.); 557-405 (s, Mg-0).
Synthesis o ~ M ~ ( O C , H ~ ) ~
Magnesium (0.15 g, 6.17 mmol) was dried in uacuo for 30 min
at 80°C. Propan-1-01 (50 m) was added and the reaction
mixture heated under reflux for 24 h. The grey-white precipi-
tate was filtered off and dried in uucuo for 3 h, giving the
product as a white powder. Yield: 90% (0.79 8). Anal. calc.:
C, 50.6; H, 9.9%. Found: C, 49.4; H, 9.3%. Mass loss in TG
for decomposition to MgO: calc.: 71.7%; found: 69.7%. IR
(KBr) v/cm-' : 2959, 2872 (s, C-H str.); 1461 (m, C-H def.);
1117, 1094 (vs, C - 0 str.); 537 (m, Mg-0).
Synthesis ofMg(0 i-C3H,)2
Diethylmagnesium (0.5 g, 6.07 mmol) was suspended in 20 ml
dry n-hexane. Propan-2-01 (4.5 ml, 59 mmol) was slowly
added. After 10 min the exothermic reaction was complete
and the mixture was stirred for another 24 h. The solvent was
removed and the white powder dried in uacuo. Yield: 96%
(0.83 8). Anal. calc.: C, 50.6; H, 9.9%. Found: C, 49.0; H, 10.1%.
Mass loss in TG for decomposition to MgO: calc.: 71.7%;
found: 70.4%. IR (KBr) v/cm-':2962, 2929, 2864, 2844 (s,
C-H str.); 1464, 1377, 1364, 1347 (m, C-H def.); 1165, 1132,
989 (vs, C - 0 str.); 883 (m, C-C str.); 582-404 (s, Mg-0).
Synthesis ofMg(OC(CH,),),
Diethylmagnesium (0.65 g, 7.88 mmol) was suspended in 50 ml
dry n-hexane. tert-Butyl alcohol (1.7 ml, 18 mmol) was then
slowly added to the mixture. After the mixture had been
stirred for 24 h, the solvent was removed under vacuum, and
the white powder dried in uucuo for 5 h. Yield: 97% (1.3 g).
Anal. calc.: C, 56.3; H, 10.6%. Found: C, 53.6; H, 11.0%.
Mass loss in TG for decomposition to MgO: calc.: 76.3%;
found: 74.0%. IR (KBr) v/cm-':2972 (s, C-H str.); 1473,
1385, 1361 (s, C-H def.); 1205 (vs, C-0 str.); 574, 499
(m, Mg-0).
Synthesis of Mg(0CH ( CH3)C6H13)2
Diethylmagnesium (0.5 g, 6.07 mmol) was suspended in 50 ml
dry n-hexane. Octan-2-01 (2.1 ml, 13 mmol) was added and
the mixture stirred for 24 h. The gelatinous product was dried
in uucuo by heating it (ca. 60-70°C) for 5 h. Yield: 93%
(1.59g). Anal. calc.: C, 68.0; H, 12.1%. Found: C, 67.3;
H, 12.5%. Mass loss in TG for decomposition to MgO: calc.:
86.8%; found: 85.9%. IR (KBr) vlcm-' : 2961, 2927, 2858 (s,
C-H str.); 1467, 1377 (s, C-H def.); 1141 (vs, C-0 str.);
586 (m, Mg-0).