A kind of analgesic medicine and its preparation method and application
A compound and crude product technology, applied in the field of analgesic drugs and their preparation, can solve the problems of lack of long-acting analgesic effect, easy to produce drug dependence, short duration of action, etc., so as to achieve improved drug application experience and long-acting analgesia. effect, the effect of reducing side effects
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Embodiment 1
[0029] Embodiment 1: Preparation of BU08028 propionate
[0030] Add 75 ml of dichloromethane and 0.01 mole of BU08028 base into a 250 ml round bottom flask under ice-cooling conditions. Mix well, and slowly add 20 mL of a dichloromethane solution containing 0.03 M triethylamine. Under the condition of rapid stirring, 20 ml of dichloromethane solution containing 0.011 mol of propionyl chloride was added dropwise. Afterwards, the mixture was stirred and reacted at room temperature for 1 hour; in the reacted mixture, 20 ml of 10% by mass sodium carbonate solution was added to neutralize the residual acid, and after the organic layer was separated, it was dehydrated using sodium sulfate, After filtration and concentration, the crude product of BU08028 propionate derivatives was obtained; the crude product of BU08028 propionate derivatives was subjected to silica gel column chromatography, and gradient elution was carried out with dichloromethane and methanol, and the volume perce...
Embodiment 2
[0032] Embodiment 2: Preparation of BU08028 valerate
[0033] Add 75 ml of dichloromethane and 0.01 mole of BU08028 base into a 250 ml round bottom flask under ice-cooling conditions. Mix well, and slowly add 20 mL of a dichloromethane solution containing 0.03 M triethylamine. Under the condition of rapid stirring, 20 ml of dichloromethane solution containing 0.011 mol of valeryl chloride was added dropwise. Afterwards, the mixture was stirred and reacted at room temperature for 1 hour; in the reacted mixture, 20 ml of 10% by mass sodium carbonate solution was added to neutralize the residual acid, and after the organic layer was separated, it was dehydrated using sodium sulfate, After filtration and concentration, the crude product of BU08028 valerate was obtained; the crude product of BU08028 valerate was subjected to silica gel column chromatography, and gradient elution was carried out with dichloromethane and methanol, and the volume percentage of methanol was from 1% to...
Embodiment 3
[0035] Embodiment 3: the preparation of BU08028 adipate
[0036]The preparation of BU08028 adipate can be prepared according to the method described in Example 1, except that 0.006 mol of adipate chloride is used instead of propionyl chloride. BU08028 adipate was tested by NMR, the results are as follows:
[0037] 1H-NMR (400MHz, CDCl 3 ): 6.64(d, 2H, J=8.0Hz), 6.55(d, 2H, J=8.0Hz), 4.32(s, 2H), 3.24(s, 6H), 2.91-2.71(m, 6H), 2.32 -2.25 (m, 12H), 1.80-1.53 (m, 12H), 1.35-0.20 (m, 52H).
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