Water → HCID 86585682, compound

Participants

Reaction Steps

1.48 g (0.0067 mol) of bis-(2-methoxyethyl)aminosulfur trifluoride is used in 10 mL of dichloromethane and within 20 minutes at 15° C.-20° C., a solution of 2.09 g of 5g in 65 mL of dichloromethane is added dropwise. The mixture is stirred for 20 hours at ambient temperature, cooled to 0° C., and carefully combined with 80 mL of water with thorough stirring. The mixture is then carefully adjusted to pH 8 with aqueous NaHCO3 solution, the organic phase is separated off, the aqueous phase is again extracted with dichloromethane, the combined organic phases are washed with water, dried over MgSO4, and evaporated to dryness. The hydrochloride is precipitated and recrystallized from acetonitrile/diethylether. Yield: 1.20 g of white crystals (53% of theory); melting point: 136° C.-137° C.

Provenance & Evidence