Preparation method of terbutaline
A technology of terbutaline and chemical equation, applied in the field of preparation of terbutaline, can solve the problems such as that the antioxidant problem cannot be well solved, will not be significantly improved, and the purity of terbutaline is low. , to reduce environmental pressure, reduce polarity, and achieve the effect of high purity
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Embodiment 1
[0030] Embodiment 1: a kind of preparation method of terbutaline
[0031] Including the following steps:
[0032] S1. Add 10 kg of compound I (65.72 mol) and 30 L of dichloromethane into the reactor, stir and dissolve, add 8.55 kg of propionic anhydride (65.72 mol), control the reaction temperature and stir at 10°C for 10 h;
[0033] S2. After the reaction is completed, add 10% diisopropylethylamine aqueous solution to the system, stir and wash thoroughly, collect the dichloromethane phase, and distill under reduced pressure to obtain 18.44 kg of yellow oil compound II (96% yield);
[0034] S3. Add 18.44kg compound II (63.08mol) and 35L ethyl acetate, 4.61kg tert-butylamine (63.08mol), 2.52kg sodium hydroxide (63.08mol) and sodium thiosulfate (63.08mol) in the reactor, control reaction The temperature was stirred and reacted at 10°C for 8h;
[0035] S4. After the reaction is completed, add purified water to the system to wash the reaction solution, collect the ethyl acetate ...
Embodiment 2
[0038] Embodiment 2: a kind of preparation method of terbutaline
[0039] Including the following steps:
[0040] S1. Add 10kg of compound I (65.72mol) and 30L of dichloromethane into the reactor, stir and dissolve, add 51.98kg of butyric anhydride (65.72mol), control the reaction temperature at 25°C and stir for 6h;
[0041] S2. After the reaction is completed, add 20% 1-methylpiperidine aqueous solution to the system, stir and wash thoroughly, collect the dichloromethane phase, and distill under reduced pressure to obtain 18.64 kg of yellow oil compound II (97% yield);
[0042] S3. Add 18.64kg compound II (63.76mol) and 35L ethyl acetate, 46.64kg tert-butylamine (637.6mol), 7.65kg sodium hydroxide (191.28mol) and antioxidant BHT (255.04mol) in the reactor to control the reaction Stir the reaction at 40°C for 4.5h;
[0043]S4. After the reaction is completed, add purified water to the system to wash the reaction solution, collect the ethyl acetate phase, and distill under r...
Embodiment 3
[0044] Embodiment 3: a kind of preparation method of terbutaline
[0045] S1. Add 10kg of compound I (65.72mol) and 30L of dichloromethane into the reactor, stir and dissolve, add 122.40kg of valeric anhydride (657.2mol), control the reaction temperature at 40°C and stir for 1h;
[0046] S2. After the reaction is completed, add 30% 4-methylmorpholine aqueous solution to the system, stir and wash thoroughly, collect the dichloromethane phase, and distill under reduced pressure to obtain 17.67kg (yield 92%) of yellow oil compound II;
[0047] S3. Add 17.67kg compound II (60.46mol) and 35L ethyl acetate, 88.44kg tert-butylamine (1209.25mol), 12.09kg sodium hydroxide (302.3mol) and antioxidant BHA (483.68mol) in the reactor to control the reaction Stir the reaction at 70°C for 1 h;
[0048] S4. After the reaction, add purified water to the system to wash the reaction solution, collect the ethyl acetate phase, and distill under reduced pressure to obtain 12.40 kg of terbutaline fi...
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