Hydrogen Bromide → HCID 19434010, compound

Participants

Reaction Steps

A mixture of the product from Step A (1.56 g), 48% HBr(16 mL) and water (4 mL) was heated at reflux temperature for 18 h, evaporated to dryness, mixed with a saturated solution of sodium bicarbonate (60 mL) and extracted with ethyl acetate (2×80 mL). The combined extracts were dried (MgSO4) and evaporated to a residue which was purified by column chromatography (silica, 5% methanol/methylene chloride) to give a firm foam (0.85 g, 56%): mp 104°-108° C. Analysis. Calculated for C13H19N3O6S3 - 0.3H2O: C, 37.63; H, 4.76; N, 10.13. Found: C, 37.61; H, 4.60; N, 10.00.

Provenance & Evidence