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5. Preparation of 3a. n-Butyllithium (20.0 ml of a 1.8 M solution in hexane, 36 mmol) was added dropwise to a stirred solution of HFC-134a (600 ml, 25 mmol) in THF (30 ml) at −78°C. After 1 h, trimethylsilyl chloride (2.3 ml, 18 mmol) was added dropwise, then 1 h later, n-butyllithium (11.0 ml of a 1.8 M solution in hexane, 20 mmol) was added dropwise. The reaction was stirred at −78°C for 1 h and then warmed to −30°C, then quenched after 30 min with saturated aqueous ammonium chloride. Extractive work-up and concentration then filtration though an alumina column (Brockmann, activity 1) eluting with pentane afforded silane 3a (2.82 g, 81%) as a colourless oil. Preparation of 5a. TASF (0.43 g, 1.4 mmol) was added gradually to a stirred solution of silane 3a (1.3 g, 7.0 mmol) and benzaldehyde (0.82 ml, 7.7 mmol) in THF (14 ml) at −30°C under argon over 24 h. Dilute HCl (15 ml of a 1 M solution, 2.1 equiv.) was added and the mixture was stirred for 15 min before extractive work-up. Column chromatography (Rf 0.26, 10% diethyl ether, 90% petroleum ether) and recrystallisation from diethyl ether/hexane afforded 5a (0.74 g, 51%) as white needles, mp 52–53°C.