Sodium Carbonate → HCID 12811241, compound

Participants

Reaction Steps

To a solution of 7 (5 g, 0.025 mol) in CHCl3 (200 ml) was added dropwise a solution of Br2 (1.3 mol, d=3.1, 4.0 g, 0.25 mol) in 100 ml CHCl3. After the addition, the solution was stirred at room temperature for 5 h, poured onto saturated Na2CO3 solution, and separated. The aqueous layer was extracted with CHCl3 (3 x). The organic layers were dried, filtered and concentrated to dryness. The residue was chromatographed on silica gel and the product eluted with CHCl3 to yield 4.4 g (65%) of 8. An analytical sample was prepared by crystallization from petroleum ether-CHCl3, m.p. 177°-178° C.

Provenance & Evidence