| Autor: |
Shen, Zheng, Ge, Jilong, Chen, Jian, Sun, Baiwang |
| Předmět: |
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| Zdroj: |
Organic Preparations & Procedures International; 2023, Vol. 55 Issue 6, p549-554, 6p |
| Abstrakt: |
In this way, intermediate B 3 b is formed by the cyclization reaction of B 1. b Next, B 3 b and B 2 b are subjected to a condensation reaction to obtain the crude paliperidone ( B 4 b ). The resulting solid was collected by suction filtration and dried at 60 ± 5 °C to afford 11.08 g (59%) of B 4 b as an off-white solid which may be further purified by activated carbon and a solution of tetrahydrofuran and purified water, as below. Unfortunately, this impurity will participate in the subsequent reaction, the corresponding impurity generated is difficult to remove, and repeated recrystallization is required to obtain a satisfactory product.[14] In our hands, we found that this step can use I tert i -butanol and potassium hydroxide aqueous solution as the reaction solvent, and compound B 1 b is cyclized at about 60 °C in this system; after the reaction, the I tert i -butanol and aqueous solution will be layered; most of the product is in the I tert i -butanol phase. After completion of the reaction, the reaction mixture was immediately suction filtered, and the solid was rinsed with 50 g of purified water. [Extracted from the article] |
| Databáze: |
Complementary Index |
| Externí odkaz: |
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