Reaction #3023143
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09034900B2
Conditions: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: To a solution of 2,6-dibromo-4-methylsulfonylphenol (1 g, 3.30 mmol) in pyridine (40 mL) was added ethynylcyclopropane (240 mg, 3.64 mmol) and Cu2O (260 mg, 1.82 mmol). The reaction mixture was degassed with N2. The mixture was heated to 130° C. for 3 hours. It was then concentrated and purified by column chromatography (PE to PE/EA=3/1) to give the title product (510 mg, 53%) as a gray solid. 1H NMR (CDCl3, 400 MHz) δ 7.99 (s, 1H), 7.93 (s, 1H), 6.52 (s, 1H), 3.07 (s, 3H), 2.13-2.11 (m, 1H), 1.13-1.05 (m, 4H). The reaction mixture was degassed with N2 It was then concentrated purified by column chromatography (PE to PE/EA=3/1)
Source ID: ord-ffe0f95e73274d279005e4d7125c97eb