Hydrochloric Acid → HCID 86651762, compound

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Reaction Steps

Hydrochloric acid (0.7 g; 38 wt. % solution) is added to DCHPOCHS-Na (1.5 g; 3.8 mmoL) in ethanol (20 mL), and the mixture is stirred for 30 minutes. Then, the ethanol is evaporated, and the residue is dried in vacuum. Dichloromethane (20 mL) and triethylorthoacetate (1.85 g; 11.4 mmoL) are added to the residue, and the resulting mixture is stirred under reflux for 10 hours. The mixture is then washed with saturated sodium bicarbonate (15 mL), then water, and then dried with sodium sulfate. The organic solvent and excess reagent are removed. The residue obtained therefrom is dried in vacuum for 1 hour to yield Ethyl 3-(dicyclohexylphosphinyl)-cyclohexane-1-sulfonate (DCHPOCHS-Et). Yield: 1.36 g (89%) 31P{1H} NMR(C6D6, ppm): 51.28 (major) and 49.24 (minor).

Provenance & Evidence