反应 #3281895
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05120859
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The alcohol 34 (5.34 g, 16.7 mmol) and CBr4 (16.6 g, 50 mmol) were dissolved in 100 mL dichloromethane and solid triphenylphosphine (13.1 g, 50 mmol) was added over a 10 min period. This solution was allowed to stir for 18 h then worked up and purified as for the synthesis of 4a. This gave 4.73 g (74% yield) of the title compound. This material crystallized on standing to give material of m.p.=87°-88° C. (Et2O/hexane). 1H NMR (CDCl3) δ 1.35/1.46 (2s, 9H), 2.41 (m, 1H), 2.58 (m, 1H), 3.90 (m, 2H), 4.48 (m, 2H), 5.19 (m, 2H), 7.34 (s, 5H). purified as for the synthesis of 4a
来源 ID: ord-4f340fc51167440a9cbea29bb13e0bdd