Preparation method and preparation intermediate of fingolimod hydrochloride
A technology for fingolimod hydrochloride and an intermediate, which is applied in the field of pharmaceutical synthesis, can solve the problems of column purification, complicated operation, low yield and the like, and achieves the effects of easy industrial production, advanced preparation technology and cost reduction.
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[0032] Example one
[0033] step 1
[0034] In a 250mL three-necked flask, add 19g (0.1mol) n-octylbenzene, 13.3g (0.1mol) aluminum trichloride, 35mL dichloromethane, cool to -10℃, drop 11.3g (0.1mol) chloroacetyl chloride to dissolve in A solution of 30 mL of dichloromethane was added at a temperature between 0° C., and after the addition was completed, stirred at room temperature for 2 hours. Pour the reaction solution into 200 mL ice water with stirring, separate the organic phase, extract the aqueous phase with 50 mL dichloromethane, combine the organic phases, wash twice with water, dry with anhydrous magnesium sulfate, filter and concentrate, and add 30 mL petroleum ether to the residue Place it in the refrigerator overnight, and filter the precipitated solid to obtain 17 g of white solid (Compound A).
[0035] Step 2
[0036] In a 500mL three-necked flask, add 200mL of absolute ethanol, cut 4.6 (0.2mol) g of metallic sodium into small pieces and slowly add them to the absolut...
Example Embodiment
[0048] Example two
[0049] step 1
[0050] In a 250mL three-necked flask, add 19g (0.1mol) n-octylbenzene, 13.3g (0.1mol) aluminum trichloride, 35mL dichloromethane, cool to -10℃, drop 11.3g (0.1mol) chloroacetyl chloride to dissolve in A solution of 30 mL of dichloromethane, the temperature of the dropwise addition is between -5-0°C, and after the dropwise addition is completed, stir at room temperature for 2 hours. Pour the reaction solution into 200 mL ice water with stirring, separate the organic phase, extract the aqueous phase with 50 mL dichloromethane, combine the organic phases, wash twice with water, dry with anhydrous magnesium sulfate, filter and concentrate, and add 30 mL petroleum ether to the residue Place it in the refrigerator overnight, and filter the precipitated solid to obtain 17.2 g of white solid (Compound A).
[0051] Step 2
[0052] In a 500mL three-necked flask, add 200mL of absolute ethanol, cut 4.6 (0.2mol) g of metallic sodium into small pieces and slow...
Example Embodiment
[0064] Example three
[0065] step 1
[0066] In a 250mL three-necked flask, add 19g (0.1mol) n-octylbenzene, 13.3g (0.1mol) aluminum trichloride, 35mL dichloromethane, cool to -10℃, drop 11.3g (0.1mol) chloroacetyl chloride to dissolve in A solution of 30 mL of dichloromethane, the temperature of the dropwise addition is between -10 and 5°C, after the dropwise addition is completed, stir at room temperature for 2 hours. Pour the reaction solution into 200 mL ice water with stirring, separate the organic phase, extract the aqueous phase with 50 mL dichloromethane, combine the organic phases, wash twice with water, dry with anhydrous magnesium sulfate, filter and concentrate, and add 30 mL petroleum ether to the residue Place it in the refrigerator overnight, and filter the precipitated solid to obtain 17.3 g of white solid (Compound A).
[0067] Step 2
[0068] In a 500mL three-necked flask, add 200mL of absolute ethanol, cut 4.6 (0.2mol) g of metallic sodium into small pieces and s...
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