反应 #3225569
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07253196B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: DMF (a few drops) was added to a mixture of 1-bromocyclopentanecarboxylic acid (23.9 g, 124 mmol) and oxalyl chloride (11.6 mL, 130 mmol) in 250 mL of CH2Cl2. The mixture was stirred at ambient temperature for 2 h. After removing the low-boiling solvents in vacuo, ethanol (50 mL) was added to the residue followed by the addition of N,N-diisopropylethylamine (22.7 mL, 130 mmol). The mixture was stirred at ambient temperature for 20 min. After removing the low-boiling solvents in vacuo, the residue was partitioned between diethyl ether and water. The organic portion was washed with water and brine, and conc. in vacuo. The crude product was filtered through a plug of silica gel using 0 to 10% EtOAc in hexanes as the eluant. The title compound was obtained as a pale oil. After removing the low-boiling solvents in vacuo, ethanol (50 mL) was added to the residue The mixture was stirred at ambient temperature for 20 min After removing the low-boiling solvents in vacuo the residue was partitioned between diethyl ether and water The organic portion was washed with water and brine The crude product was filtered through a plug of silica gel using 0 to 10% EtOAc in hexanes as the eluant
来源 ID: ord-a81deba6fbbe4eee8285d8bc265b95ef