Synthesis of quetiapine and pharmaceutically acceptable salts thereof
A mixture, hemi-fumarate technology, applied in the direction of active ingredients of heterocyclic compounds, organic chemistry, etc., can solve problems such as long reaction time
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Embodiment 1
[0041] Reagent
[0042] 11-piperazinyldibenzo[b,f][1,4]thiazepane hydrochloride 2.75 g (7.5 mmol)
[0043] 1.2 g (9.6 mmol) of 2-(2-chloroethoxy)ethanol
[0044] Na 2 CO 3 4.75 g (45 mmol)
[0045] NaI 40-50 mg (about 0.3 mmol)
[0046] n-Butanol 15ml
[0047] TBAB 0.5g
[0048] process
[0049] The reagents were added to a round bottom flask and heated to 115°C-120°C under gentle reflux for 24 hours. Heating was discontinued, the solution was cooled, and the resulting slurry was filtered. The precipitate was washed twice with a small amount of butanol. The washings were combined with the filtrate, and the precipitate was discarded. Fumaric acid (0.435 g, 3.75 mmol) was added to the filtrate, the mixture was heated on a boiling water bath, the flask was removed from the water bath, and quindipine hemifumarate crystallized. The precipitate was collected (isolated) by filtration and recrystallized from 28 mL of ethanol to give 2.0 g of product (60.4%).
Embodiment 2
[0051] Reagent:
[0052] 11-piperazinyldibenzo[b,f][1,4]thiazepane hydrochloride 5.5 g (15 mmol)
[0053] 2-(2-Chloroethoxy)ethanol 2.4 g (19 mmol)
[0054] Na 2 CO 3 9.5 g (90 mmol)
[0055] NaI 90 mg (0.6 mmol)
[0056] 30ml n-butanol
[0057] TBAB 1 g
[0058] process:
[0059] The reagents were added to a round bottom flask equipped with a magnetic stirrer and a condenser with a calcium chloride drying tube. Place the flask in an oil bath at 115-120°C and stir the contents of the flask under gentle reflux conditions. After 24 hours of heating, the heating was stopped and the mixture was cooled and filtered. The precipitate was collected on a Buchner filter, washed twice with butanol, the washings were combined with the filtrate, and the precipitate was discarded. The filtrate was added to a reaction vessel, and fumaric acid (870 mg, 7.5 mmol) was added to the vessel, and the mixture was heated to boiling on an oil bath. The container was removed from the oi...
Embodiment 3
[0061] Reagent:
[0062] 11-piperazinyldibenzo[b,f][1,4]thiazepane hydrochloride 16.5 g (44 mmol)
[0063] 7.2 g (58 mmol) of 2-(2-chloroethoxy)ethanol
[0064] Na 2 CO 3 28.5 g (270 mmol)
[0065] NaI 270 mg (0.18 mmol)
[0066] TBAB 3 grams
[0067] Toluene 82.5ml
[0068] process:
[0069] The reagents were added to a round bottom flask equipped with a magnetic stirrer and a condenser with a calcium chloride drying tube. The flask and contents were heated in an oil bath at 105°C under gentle reflux. After heating for 24 hours, a Dean Stark trap was attached to the flask and an azeotropic mixture of water and toluene was distilled off. The product remaining in the flask was filtered off. The precipitate (salt) was washed with a small amount of toluene on a Buchner filter, the washings were combined with the filtrate, and the precipitate was discarded.
[0070] To the filtrate contained in the flask was added 2.6 g (22 mmol) of fumaric acid, the mixture was he...
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