Preparation method for lormetazepam rearrangement product
A technology of chlormetazepam and rearrangement, applied in the direction of organic chemistry, etc., can solve the problems of using highly toxic reagents, too long preparation steps, and polluting the environment, and achieve the effects of simple post-processing, high reaction safety, and high yield
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Embodiment 1
[0020] The preparation method of chlormetazepam rearrangement product is as follows:
[0021] Add 0.1 mol of chlormetazepam to 200 mL of absolute ethanol, stir well at room temperature, then add 0.12 mol of solid sodium hydroxide, react at 20°C for 3 h, distill all the ethanol out under reduced pressure to obtain a residue, and add to the residue 200 mL of purified water was added for one wash, and after filtration, 100 mL of purified water was used for a second wash. The obtained solid was vacuum-dried at -0.08 MPa and 80° C. for 2 h to obtain 32.39 g of chlormetazepam rearrangement product. After calculation, the product yield is 97.21%, and the purity is 99.78%.
Embodiment 2
[0023] The preparation method of chlormetazepam rearrangement product is as follows:
[0024] Add 0.15 mol of chlormetazepam to 300 mL of ethyl acetate, stir well at room temperature, then add 0.225 mol of solid sodium hydroxide, react at 40°C for 3 h, distill off all the ethyl acetate under reduced pressure to obtain a residue, and transfer to the residue 200 mL of purified water was added to the mixture for one wash, and after filtration, 100 mL of purified water was used for two washes. The obtained solid was vacuum-dried at -0.08 MPa and 80° C. for 2 h to obtain 48.73 g of chlormetazepam rearrangement product. After calculation, the product yield of this embodiment is 97.5%, and the purity is 99.85%.
Embodiment 3
[0026] Add 0.2 mol of chlormetazepam to 400 mL of acetonitrile, stir well at room temperature, then add 0.36 mol of solid sodium hydroxide, react at 60°C for 1 h, distill off all the acetonitrile under reduced pressure to obtain a residue, add 200 mL of Wash once with purified water, and then wash twice with 100 mL of purified water after filtration. The obtained solid was vacuum-dried at -0.08 MPa and 80°C for 2 hours to obtain 64.91 g of the rearrangement product of chlormetazepam. After calculation, the product yield is 97.4%, and the purity is 99.67%.
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