反应 #3006282
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08067590B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To 5.00 g (37.5 mmol) aluminium(III)-chloride in 20 mL 1,2-dichloroethane is added at 0° C. dropwise 2.24 mL (28.1 mmol) 1,3-dichloro-propan-2-one keeping the temperature below 15° C. Then 4.48 g (18.7 mmol) 1-(1,3-dihydro-isoindol-2-yl)-2,2,2-trifluoro-ethanone in 5 mL 1,2-dichloroethane is added dropwise at RT keeping the temperature between 40-45° C. The reaction is stirred for 18 h at RT and is poured onto aqueous HCl-solution. The aqueous phase is extracted twice with DCM, the organic phase is washed with water, dried over MgSO4, filtered and the solvent is evaporated. The residue is elutriated with PE and the precipitate is collected. between 40-45° C The aqueous phase is extracted twice with DCM the organic phase is washed with water dried over MgSO4 filtered the solvent is evaporated the precipitate is collected
来源 ID: ord-c7a062b9fb2246018f4a28707b8cd444