Method for preparing n-ethyl-l-menthyl formamide by inverting configuration of n-ethyl-neo-menthyl formamide
A technology of menthyl formamide and configuration inversion, applied in the field of configuration inversion of fine chemicals, can solve the problem of increasing equipment investment and production cost, increasing separation difficulty, and increasing the total yield of N-ethyl-L-menthyl formamide. The problem of unsatisfactory rate and other problems can achieve the effect of convenient post-reaction treatment, lower energy consumption and lower production cost.
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Embodiment 1
[0027] N- ethyl - New - menthyl carboxamide with N- ethyl carboxamide -L- menthyl mixture 30g (N- ethyl - New - menthyl carboxamide / N- ethyl carboxamide menthyl = -L- 0.38) was dissolved in 150ml of toluene was added 0.6gN, N'- dicyclohexylmethylamine to the system. Under nitrogen blanket with stirring at conditions of 135 ℃ 24h. After washing twice with water after cooling water was added to the reaction system (wash to pH between 7 and 7.5), allowed to stand waiting layers were separated and the organic layer was removed and then the amount of delamination, delamination was allowed to stand again the organic layer was removed under reduced pressure to recover the solvent toluene was distilled off, to obtain about 27.4g product, the GC internal standard: N- ethyl - new - menthyl carboxamide / N- ethyl carboxamide menthyl = -L- 0.02, conversion was 91.3%, the selectivity 99.3%.
Embodiment 2
[0029] N- ethyl - New - menthyl carboxamide with N- ethyl carboxamide -L- menthyl mixture 30g (N- ethyl - New - menthyl carboxamide / N- ethyl carboxamide menthyl = -L- 0.26) was dissolved in 150ml of toluene was added 0.6gN, N'- dicyclohexyl-ethylamine to the system. Under nitrogen blanket with stirring at conditions of 135 ℃ 24h. Suitable water was added after cooling the reaction system which was washed with water until a pH of between 7 and 7.5, allowed to stand waiting stratification, the organic layer was removed and the layers were separated and washed twice with an appropriate amount of water, layered again, remove the organic recovering the toluene layer was distilled off under reduced pressure, to obtain about 28.5g product, GC internal standard quantification: N- ethyl - new - menthyl carboxamide / N- ethyl carboxamide -L- menthyl = 0.01, conversion was 95%, the selectivity was 99.1%.
Embodiment 3
[0031] N- ethyl - New - menthyl carboxamide with N- ethyl carboxamide -L- menthyl mixture 50g (N- ethyl - New - menthyl carboxamide / N- ethyl carboxamide menthyl = -L- 0.38) were dissolved in 250ml of toluene was added to the system 2.5gN, N'- diisopropylethylamine. Under nitrogen blanket with stirring at conditions of 135 ℃ 24h. The filtrate was added to pure water to a pH of between 7 and 7.5, allowed to stand waiting stratification, the organic layer was removed and the layers were separated and washed twice with an appropriate amount of purified water, allowed to stand again separated and the organic layer was removed under reduced pressure conditions recovering the toluene was distilled, to obtain about 46.7g product, the GC internal standard: N- ethyl - new - menthyl carboxamide / N- ethyl carboxamide -L- menthyl = 0.025, the conversion was 93% and the selectivity 98.9%.
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