反应 #3737663
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05817890
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 7 g (175 mmol) of sodium hydroxide pellets were added in three portions at 10°-15° C. to 15.2 g (63.88 mmol) of 2,2,6,6-tetrachlorocyclohexanol 1a in suspension in 70 cm3 of distilled water. The reaction mixture was kept at room temperature for 1 h 15 min, 20 cm3 of ethyl ether were then added, stirring was continued for 5 min and then the phases were separated and the aqueous phase was extracted with ether (6×50 cm3). The ether phases were combined, dried over MgSO4, filtered, and the mixture was concentrated with a rotary evaporator. A liquid epoxide 2a (m=12.42 g) was obtained, representing 96.5% of the theoretical yield. The compound 2a will be frequently employed without further purification in the following stages (semicapillary GC purity>96%). The epoxide 2a can be purified by distillation at reduced pressure (boiling at 40° C. at 0.1 mm Hg); after distillation, the yield of compound 2a was 92%. was continued for 5 min the phases were separated the aqueous phase was extracted with ether (6×50 cm3) dried over MgSO4 filtered the mixture was concentrated with a rotary evaporator
来源 ID: ord-16bcfe4dac324138b23b04b0ca147210