반응 #69622
ord-00b8032a959e4335b0845a1c12a5a3f9
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후처리
- 1기타at room temperature
- 2기타(25° C.)
- 3기타for 5 min
- 4기타the pre-preparation of a rearrangement catalyst
- 5기타After the pre-preparation, high performance liquid chromatography analysis
- 6기타had been consumed
- 7workup.DISSOLUTIONthe materials were dissolved
- 8workup.ADDITION1 molar ratio was added
- 9기타which then reacted for 60 min
실험 절차
Within a glove box, 0.033 g (0.17 mmol) of cyclododecanone oxime prepared in Reference Example 2 was dissolved in 0.400 g of a 5% by weight thionyl chloride (rearrangement catalyst)/toluene solution (0.020 g (0.17 mmol) as pure thionyl chloride), and the mixture was stirred using a magnetic stirrer at room temperature (25° C.) for 5 min, to conduct the pre-preparation of a rearrangement catalyst. After the pre-preparation, high performance liquid chromatography analysis indicated that cyclododecanone oxime had been consumed. Separately, within a glove box (under nitrogen atmosphere), in a flat-bottom flask equipped with a manifold, 3.285 g (16.64 mmol) of cyclododecanone oxime and 0.023 g (0.17 mmol) of zinc chloride were weighed and then 7.00 g of toluene was added, and the materials were dissolved by heating the mixture to 100° C. in an oil bath. To the zinc-chloride containing solution of cyclododecanone oxime in toluene, the reaction mixture which had been prepared in the pre-preparation using cyclododecanone oxime and thionyl chloride in 1:1 molar ratio was added, which then reacted for 60 min. The reaction solution was clear without turbidity, and gas chromatography analysis indicated that a conversion of cyclododecanone oxime was 100% and a laurolactam yield was 98.8%.