Process for synthesizing Tuoteluodin L-tartrate
A synthesis method and tartaric acid technology are applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., and can solve the problems of anti-muscarinic side effects, difficulty in eye adjustment, serious side reactions, etc., and reduce side effects, The effect of rapid absorption and short response time
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Embodiment 1
[0012] Preparation of 6-methyl-4-phenyl-3,4-dihydrocoumarin [I]
[0013] Cinnamic acid (74g, 0.5mol), p-methylphenol (54g, 0.5mol), and concentrated sulfuric acid (20ml) were mixed, heated to 120-125°C, stirred for 1 hour, TLC (petroleum ether: ethyl acetate=4:1 ) after showing that the raw material has reacted completely, it is cooled to room temperature, and the reactant is extracted with ethyl acetate (250ml×2), the organic layer is washed with water, and anhydrous Na 2 SO 4 After drying, the ethyl acetate was evaporated to give [I] 108g, the yield was 90.8%. mp: 83-86°C, directly put into the next reaction without purification.
Embodiment 2
[0015] Preparation of 3-(2-methoxy-5-methylphenyl)-3-phenylpropanoic acid [II] [I] (71.4 g, 0.3 mol) was dissolved in 10% NaOH solution (480 ml) at room temperature Add dropwise (CH 3 ) 2 SO 4 (94.5g, 0.75mol), and vigorously stirred, and after the solution became clear, heated at 80°C for 0.5 hours, TLC (same as above), cooled, acidified with hydrochloric acid, and dried to give milky white solid [II] 68.5g (85% yield Rate), mp = 133 ~ 135 ° C, no need to purify directly into the next step reaction.
Embodiment 3
[0017] Preparation of N,N-diisopropyl-3-(2-methoxy-5-methylphenyl)-3-phenylpropanamide [III].
[0018] [II] (1 3.5g, 0.05mol) and SOCl 2 (50ml) mixed, heated to reflux and stirred for 3 hours, evaporated excess SOCl 2 , to obtain brown acid chloride, the resulting acid chloride was dissolved in dichloromethane (50ml), and added dropwise to diisopropylamine (20.2g, 0.20mol) in 100ml of dichloromethane solution at 0°C, stirred for 2-4 hours, TLC (same as above ), after distilling off the solvent, put it into ice water, filter out the solid, wash with water and dry to obtain 14 g of light yellow solid [III] with a yield of 79%.
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