反应 #3320055
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09273017B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 1-(4-hydroxy-2-trifluoromethyl-phenyl)-ethanone (29.74 g; 145.7 mmol) in CH2Cl2 (300 mL) and THF (120 mL) was added Et3N (24.4 mL; 174.8 mmol), at 0° C. To the resulting mixture was added dropwise a solution of methanesulfonyl chloride (12.5 mL; 160.3 mmol) in CH2Cl2 (60 mL), at 0° C. Subsequently the mixture was stirred overnight at RT, and poured in ice-water. The layers were separated and the organic layer was washed with 1 M aqueous HCl and water; dried (MgSO4), filtered and concentrated in vacuo to afford methanesulfonic acid 4-acetyl-3-trifluoromethyl-phenyl ester (40.47 g), which was used as such. at 0° C at 0° C The layers were separated the organic layer was washed with 1 M aqueous HCl and water dried (MgSO4) filtered concentrated in vacuo
来源 ID: ord-c06fd158857d478ba17931958e07562d