2-Bromopropane → HCID 56634327, compound

Participants

Reaction Steps

50 mg of compound (6) was dissolved in 1.0 ml of dry dimethylformamide under a nitrogen atmosphere and mixed with about 3 mg of sodium hydride under cooling with ice. After 30 minutes, 12.2 μl of 2-bromopropane was added, and the reaction solution was stirred at room temperature. The reaction solution was allowed to react for 63 hours, while about 3 mg of sodium hydride and 12.2 μl of 2-bromopropane were added after 40 hours and further after 46 hours. Then, the reaction solution was charged onto a silica gel column (Kieselgel 60, Merck, 1.0φ×30 cm) and eluted with n-hexane-ethyl acetate (2:1). The fraction containing the desired product was concentrated to dryness to give 13.6 mg of compound (33).

Provenance & Evidence