Notes- Reactions of t-Butyl Hypochlorite

Abstract

NOTES 1835 excluded. The main fraction (379 g. + 26 g. from forerun = 405 g. or 73 mole-% conversion) was I, b.p. 215°/750 mm., n2Ds 1.4550 (hydrol. chlorine, 42.3%; caled., 42.2%). ß-Cyanoethylethyldichlorosilane (III). Similar treatment of 254 g. (1.35 moles) of II with ethylmagnesium chloride prepared from 36.4 g (1.5 moles) of magnesium turnings and 97 g. (1.5 moles) of rthyl chloride in a total of 1 1. of tetrahydrofuran at -50°g ave after filtration and removal of the solvent, 205 g. of crude product. Fractional distillation gave 168 g. total (conversion, 69 mole-%) of III as the main product (hydrol. chlorine, 37.9%; caled., 38.9%) b.p. 234-235°/751 mm. and a forerun b.p. 200-234°/751 mm. (hydrol. chlorine, 34.8%) consisting of a mixture of 21.5 g. (conversion, 9 mole-%) of /3-cyanoethylchlorodiethylsilane (caled, hydrol. chlorine, 20.2%) and 5 g. of III. Silicones DivisionUnion Carbide Corporation ToNAWANDA, N. Y.