in benzene T=5 - 10°C; 1.5 h;

in benzene T=5 - 10°C; 1.5 h;

in acetonitrile Ar atm.; molar ratio TlF:(Me3SiN)2S 2:1, stirring (20°C, 24 h); evapn., drying (6 h, vac.);

in dichloromethane T=22°C; 8 h; effect of increased reagent concentration and reduced addition time on yield and volume efficiency; Product distribution;

1.) CCl4, 5-10 deg C, 2.) CH2Cl2, 22 deg C, 14 h; Yield given. Multistep reaction. Further byproducts given. Yields of byproduct given;

in hexane under Ar, Ti complex (0.706 mmol) dissolved in hexane (10 ml), N,N-bis(trimethylsilyl)sulfurdiimide added, mixt. stirred at 50°C for 5 d; amount of solvent reduced at 0°C, distilled at 70°C and 0.1 mbar to reveal 1,2,3,4-tetramethylfulvene, n-hexane, bis(trimethylsilyl)acetylene, and N,N'-bis(trimethylsilyl)sulfurdiimide, solid dissolved in n-hexane, stored at -78°C;

in diethyl ether; hexane; cyclohexane 2 h;

in neat (no solvent) exclusion of moisture; condensation of F-compd. and Si-compd. in NMR-tube (-80°C), shaking, warming (-40°C), warming (2 h, -10°C), warming (5 h, 20°C); not isolated; (1)H-NMR-spctroscopy;

in benzene T=5 - 10°C; 1.5 h;

in pentane (under exclusion of moisture); addn. of NSF to a soln. of the sulfurdiimide in pentane in a pressure-tight apparatus at -195°C, slow warming to room temp. with stirring; decanting, evapn. of the volatiles;