Method for preparing MPTF-E (meptazinol E)
A technology of mebutamol and impurities, applied in the field of chemical drug preparation, to achieve the effects of high stability, low energy consumption and high purity
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Embodiment 1
[0026] Example 1: Preparation of compound I:
[0027] Add 65mL of anhydrous THF to a 250mL three-neck flask, slowly add 11.8mL of 2,2,6,6-tetramethylpiperidine dropwise, then add 45mL of n-butyllithium (1.6M n-hexane solution), stir, and cool down to 0°C . Dissolve 8.92g of N-methylcaprolactam in 15mL of anhydrous THF, add to the above reaction solution, stir at 0°C for 10min, add 45mL of n-butyllithium (1.6M n-hexane solution), continue stirring for 10min, then add 10g of Chloroanisole. After reacting for 90 minutes, 50 mL of ice water was added, and stirring was continued for 30 minutes. The organic phase was distilled off under reduced pressure, dissolved in 100 mL ethyl acetate, washed with 4N HCl and saturated brine, and the organic phase was washed with anhydrous Na 2 SO 4 After drying and concentrating, it was purified by silica gel column chromatography to finally obtain 3.77 g of light yellow solid (yield 23.0%).
Embodiment 2
[0028] Example 2: Preparation of Compound II:
[0029] Add 50mL of anhydrous THF to a 100mL three-neck flask, slowly add 5.4mL of 2,2,6,6-tetramethylpiperidine dropwise, then add 20mL of n-butyllithium (1.6M n-hexane solution), stir, and cool down to 0°C . After reacting for 15 min, 3.73 g of compound I was added and kept stirring at 0°C for 1 h. Add 2.99g iodoethane, heat to room temperature and stir for 13h, add 100mL ice water, and continue stirring for 30min. Remove the organic phase by distillation under reduced pressure, add 100 mL of ethyl acetate to dissolve, wash with 80 mL of 4NHCl and saturated brine, and wash the organic phase with anhydrous Na 2 SO 4 After drying and concentrating, it was purified by silica gel column chromatography to finally obtain 3.12 g of a yellow oil (yield 74.7%).
Embodiment 3
[0030] Example 3: Preparation of compound III:
[0031] 0.5 g of compound II was dissolved in 15 mL of anhydrous DCM (dichloromethane), and 1.44 g of boron tribromide was dissolved in 4 mL of DCM (dichloromethane) and added to the above reaction solution. After cooling down to 0°C for 3.5 h, use saturated NaHCO 3 Adjust the pH of the solution to 5-6, separate the liquids, extract the aqueous phase with 10mL DCM, combine the organic phases, and use anhydrous NaSO 4 After drying, 0.385 g of white solid was finally obtained (yield 81.4%).
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