反应 #2075131
ord-6091efd7fcf74430a181d5af21e22915
反应方程式
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1浓缩the reaction mixture was concentrated in vacuo
- 2其他Purification of the crude residue by flash column chromatography on 80 g of silica gel (hexane→EtOAc, gradient)
实验过程
Bromine (0.47 mL, 9.12 mmol) was added to a solution of imidazole (617 mg, 9.06 mmol) and triphenylphosphine (2.40 g, 9.15 mmol) in CH2Cl2 (30 mL) at room temperature. A solution of methyl 5-hydroxymethyl-thiophene-2-carboxylate (prepared according to the procedures described in WO2004/037808; 1.30 g, 7.59 mmol) in CH2Cl2 (10 mL) was then added. After 10 min at room temperature, the reaction mixture was concentrated in vacuo. Purification of the crude residue by flash column chromatography on 80 g of silica gel (hexane→EtOAc, gradient) afforded 1.70 g (95%) of the title compound (B).