Preparation of amidated natural metha camphor as effective algefacient
A technology of cooling agent and menthol, which is applied in the field of preparation of new high-efficiency cooling agent amidated menthol, can solve the problems of development and application limitations, low conversion rate, etc., achieve better effect, increase whiteness, and reduce production cost Effect
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Embodiment 1
[0023] Preparation of N-ethyl-p-menthane-3-carboxamide
[0024] 1. Preparation of Chloromenthane
[0025] Add ZnCl to the reaction flask 2 / HCl saturated solution, introduce HCl gas under stirring, add menthol crystals, continue stirring for 2-3h, when the conversion rate (GC) reaches above 97%, the reaction ends. Distilled under reduced pressure to obtain menthane chloride with a yield of 95% and a purity of 97% (GC).
[0026] 2. Preparation of Magnesium Chloromenthane
[0027] The reaction was carried out in a reaction flask equipped with magnetic stirring. Weigh the quantitatively treated magnesium bars and add them to the reaction bottle, add anhydrous ether and initiator, stir the reaction, add dropwise the mixture composed of chloromenthane and anhydrous ether, the dropping time is about 1 hour, after the dropwise addition is completed The reaction was continued for 2-3h, and the reaction was completed, and the reaction mixture was directly used for the next reaction...
Embodiment 2
[0035] Preparation of N-tert-butyl-p-menthane-3-carboxamide
[0036] Substitute tert-butylamine for monoethylamine and follow the steps above to prepare N-tert-butyl-p-menthane-3-carboxamide with a purity of 97%, a melting point of 94-96°C and a whiteness of 94.
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