反应 #3745932
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08754106B2
反应条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of compound 75 (19 g, 0.1 mol) in quinoline (50 mL) was heated to 170° C. for 2 h (until effervescence ceased). The reaction mixture was cooled to RT and aqueous NaOH solution was added (1M, 500 mL) followed by pet. ether (500 mL). The reaction mixture was stirred for 15 min and the aqueous layer was separated. The aqueous layer was further washed with pet. ether (2×300 mL) to remove quinoline completely. The aqueous layer was acidified with 1.5N HCl to pH=5, the solid was filtered off and dried under vacuum. The obtained solid was further washed with 5% ethyl acetate in pet. ether to give pure title compound (12 g, 82%). The reaction mixture was cooled to RT the aqueous layer was separated The aqueous layer was further washed with pet. ether (2×300 mL) to remove quinoline completely the solid was filtered off dried under vacuum The obtained solid was further washed with 5% ethyl acetate in pet. ether
来源 ID: ord-4040c5294c004dd394ec8a4c74333a12