反应 #1785070
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08592456B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of (E)-2-chloro-6-fluorobenzaldehyde oxime (2 g) in 10 mL Dimethylformamide (DMF) at room temperature 0.23 g N-Chlorosuccinimide (NCS) were added. Dry hydrogen chloride was bubbled into the DMF solution until the reaction temperature rise up to 35° C. Then 1.21 g N-chloro-succinimide were added in portions, the temperature was kept at 35-45° C. The reaction mixture was cooled to room temperature and poured into 30 mL ice and extracted with ether. Combined extracts were dried and evaporated to give 2.5 g of 2-chloro-6-fluoro-N-hydroxybenzimidoyl chloride as a yellow oil. Dry hydrogen chloride was bubbled into the DMF solution until the reaction temperature rise up to 35° C Then 1.21 g N-chloro-succinimide were added in portions was kept at 35-45° C poured into 30 mL ice extracted with ether Combined extracts were dried evaporated
来源 ID: ord-eeb1ec58b9d94bbaad975e33a2f8b30a