1: isopropenyl bromide With tert.-butyl lithium in diethyl ether T=-78°C; 3 h; 2: tributyltin chloride in diethyl ether T=-78 - 20°C; 16 h;

in tetrahydrofuran

Burgess Reagent in benzene byproducts: HNEt3(1+)*OSO2NHCO2Me(1-); addn. of alcohol to the inner salt under inert atm., room temp., soln. stirred overnight, heated (70°C, 6 h), hydrolyzed; chromy. (florisil, pentane);

sodium hydrogen sulphate; sulfuric acid; water in pyridine; dichloromethane byproducts: p-H3CC6H4OH; slow addn. of soln. of CH3PhOC(S)Cl in CH2Cl2 to cold (-20°C) soln. of alcohol in pyridine, 3h. 0°C, ice, extd. with CH2Cl2, treatment with H2SO4 (10percent), NaHCO3 (10percent), H2O; mixt. warmed up to 200°C, then thermolysis at 800°C; in N2, condensation of products in a dewar vessel (liquid N2), warmed up to ambient temp.; first reaction detected by HPLC and IR, purifn. of educt by chromy. (Florisil, pentane), purifn. checked by HPLC or GC;

React. of starting materials at -100°C for 1 h.; Mixt. is allowed to warm to 0°C over 1 h, and quenched with MeOH at -100°C.;

n-butyllithium in tetrahydrofuran; hexane to a stirred soln. of phosphonium-compd. in THF at 0°C is added a soln. of BuLi in hexane under N2, the mixt. is stirred at room temp. for 1 h and recooled to 0°C, addn. of Sn-compd. and the mixt. is stirred for 12 h, addn. of aq. NH4Cl; extraction with light petroleum, the extract is dried (MgSO4) and evaporated under reduced pressure, purifn. by column chromy. on silica gel (elution with pentane);

n-butyllithium; ammonium chloride (Ar); Soln. of (Bu)3SnLi in THF added by syringe to stirred suspensn. of CuCN in THF at -78 °C, mixt. stirred during 30 min at this temp.; further 30 min react. on CO2/acetone bath with allene; slow warming to 0 °C; satd. NH4Cl added; extractn. (Et2O); drying (MgSO4); chromy.;

in gas byproducts: hexabutylditin; placing starting material in a porcelain cup in the sublimation chamber of a flash vac. thermolysis apparatus, react. at 800-850°C in the main oven and 250-300°C in the sublimation oven (10E-2 mm), oven packed with broken porcelain; vapors quenched on a dewar cold finger, pyrolysis tube cooled to room temp., product washed with ether from the dewar surface, ether evapd., chromy. (florisil);

in gas byproducts: hexabutylditin; placing starting material in a porcelain cup in the sublimation chamber of a flash vac. thermolysis apparatus, react. at 800-850°C in the main oven and 250-300°C in the sublimation oven (10E-2 mm), oven packed with broken porcelain; vapors quenched on a dewar cold finger, pyrolysis tube cooled to room temp., product washed with ether from the dewar surface, ether evapd., chromy. (florisil);

in gas byproducts: hexabutylditin; placing starting material in a porcelain cup in the sublimation chamber of a flash vac. thermolysis apparatus, react. at 800-850°C in the main oven and 250-300°C in the sublimation oven (10E-2 mm), oven packed with broken porcelain; vapors quenched on a dewar cold finger, pyrolysis tube cooled to room temp., product washed with ether from the dewar surface, ether evapd., chromy. (florisil);