Boron trifluoride etherate → HCID 15123251, compound

Participants

Reaction Steps

A solution of the product of Example 8 (0.25 g) and ethanedithiol (0.1 ml) in dry dichloromethane (5 ml) at 0°-5° was treated with borontrifluoride etherate (0.020 ml, 0.16 mmol). The mixture was stirred at ambient temperature for 18 h. Aqueous sodium hydroxide (2M; 5 ml) was added and the product was extracted with dichloromethane (2×15 ml). The combined extracts were dried and evaporated to give an oily residue, which was purified by flash chromatography eluting with dichloromethane/methanol/ammonia 200:8:1 to give a solid which was crystallized from a mixture of methylacetate and hexane to give the title compound as a solid (0.155 g) m.p. 119°-20°. T.l.c. SiO2Dichloromethane/methanol/ammonia 150:10:2 Rf 0.7.

Provenance & Evidence