A kind of preparation method of the butoconazole nitrate intermediate suitable for industrialized production
A technology for butoconazole nitrate and intermediates, which is applied in the field of preparation of butoconazole nitrate intermediates, can solve the problems of personnel damage and equipment damage, difficult control of Grignard reaction, ether volatilization, etc., so as to reduce side reactions and increase operability Sexuality and safety, the effect of increasing feasibility
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Embodiment 1
[0031] 1. Grignard reaction: In a 20L dry reaction kettle, add 504g (21mol) of magnesium powder, 6.4L of anhydrous methyl tert-butyl ether and tetrahydrofuran (volume ratio 15:1) mixed solvent and a catalytic amount of iodine in sequence at room temperature , under stirring, first drop 0.6-0.8L of anhydrous methyl tert-butyl ether solution (4L in total) containing 3.22kg (20mol) of p-chlorobenzyl chloride, and stir until the reaction is initiated (the solution becomes cloudy and the temperature rises), and the temperature Raise to about 40°C, continue to add the remaining solution, keep at 40-50°C, drop for about 1-2 hours, and keep warm for 1-2 hours.
[0032] 2. Condensation reaction: the above reaction system is lowered to room temperature, and directly dropwise add 1.85kg (20mol) of epichlorohydrin 4L solution of anhydrous methyl tert-butyl ether to the reaction kettle under stirring, control the dropping rate and maintain the temperature At about 40°C, drop it in about 1 ...
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Description
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Application Information
- IPC
- C07C33/46; C07C29/64
- CPC
- C07C29/64; C07F3/02; C07C33/46
- Inventors
- 郑德强; 王长斌