Synthesis method of vitamin B6 triisopalmitate

Abstract

The invention is suitable for the field of chemical synthesis, and provides a synthesis method of vitamin B6 triisopalmitate. The method comprises the following steps: mixing vitamin B6 hydrochloride,pyridine and cyclohexane, carrying out ice bath treatment, dropwisely adding 2-hexyldecanoyl chloride, and carrying out a heat preservation reaction to obtain a reaction solution; carrying out standing layering treatment on the reaction solution, and taking the upper layer to obtain an upper-layer solution A; adding an oxalic acid aqueous solution into the upper-layer solution A, layering, and taking the upper layer to obtain an upper-layer solution B; adding petroleum ether and a saturated sodium bicarbonate solution into the upper-layer solution B, layering, adding a saturated sodium chloride solution, and washing to obtain a clarified solution; and adding a calcium carbonate viscous liquid into the clarified solution, carrying out stirring and liquid separation, adding activated carbon, and purifying to obtain the vitamin B6 triisopalmitate. The synthesis method provided by the invention is simple in reaction, the obtained product is high in purity, and less wastewater, waste gas and waste residues are generated, so that the method is beneficial to the environment.

Description

technical field

[0001] The invention belongs to the field of chemical synthesis, in particular to a synthetic method of vitamin B6 triisopalmitate. Background technique

[0002] Vitamin B6 triisopalmitate is a common pharmaceutical intermediate and industrial raw material, which is generally synthesized from vitamin B6 (Vitamin B6).

[0003] However, the traditional synthetic method of vitamin B6 triisopalmitate is relatively complicated, and the price of the raw materials used is unstable, and it is easy to produce more waste gas, waste water and waste residue, which is not good for the environment. Therefore, it is urgent to study a low-cost A cost-effective and environmentally friendly synthesis method of vitamin B6 triisopalmitate. Contents of the invention

[0004] The purpose of the embodiments of the present invention is to provide a synthetic method of vitamin B6 triisopalmitate, aiming to solve the problems raised in the background technology.

[0005] The embod...

Examples

Embodiment 1

[0024] This embodiment provides a kind of synthetic method of vitamin B6 triisopalmitate, it comprises the following steps:

[0025] (1) 1mol of vitamin B6 hydrochloride, 5mol of pyridine and 7mol of cyclohexane were mixed for 30min, and placed in an ice bath at a temperature of 15°C, then 2mol of 2-hexyldecanoyl chloride was added dropwise ( Control the dropwise addition within 4h) to carry out the heat preservation reaction for 24h to obtain the reaction solution.

[0026] (2) Pour the reaction solution into a separatory funnel and carry out static layering treatment for 0.1h, then take the upper layer to obtain the upper layer A.

[0027] (3) Add an aqueous oxalic acid solution with a mass concentration of 1% to the supernatant A for stratification, and take the upper layer to obtain a supernatant B; wherein, the molar mass of oxalic acid in the oxalic acid aqueous solution is 2 mol.

[0028] (4) After adding 2mol sherwood oil and saturated sodium bicarbonate solution to l...

Embodiment 2

[0031] This embodiment provides a kind of synthetic method of vitamin B6 triisopalmitate, it comprises the following steps:

[0032] (1) 1mol of vitamin B6 hydrochloride, 7mol of pyridine and 9mol of cyclohexane were mixed for 30min, and placed in an ice bath at a temperature of 5° C., then added dropwise with 4mol of 2-hexyldecanoyl chloride ( Control the dropwise addition within 4h) to carry out the heat preservation reaction for 24h to obtain the reaction solution.

[0033] (2) Pour the reaction solution into a separatory funnel for static layering treatment for 1 h, then take the upper layer to obtain the upper layer A.

[0034] (3) Add an aqueous oxalic acid solution with a mass concentration of 3% to the supernatant A for stratification, and take the upper layer to obtain a supernatant B; wherein, the molar mass of oxalic acid in the oxalic acid aqueous solution is 4mol.

[0035] (4) After adding 4mol sherwood oil and saturated sodium bicarbonate solution to layering in...

Embodiment 3

[0038] This embodiment provides a kind of synthetic method of vitamin B6 triisopalmitate, it comprises the following steps:

[0039] (1) 1mol of vitamin B6 hydrochloride, 6mol of pyridine and 8mol of cyclohexane were mixed for 30min, and placed in an ice bath at a temperature of 10°C, then 3mol of 2-hexyldecanoyl chloride was added dropwise ( Control the dropwise addition within 4h) to carry out the heat preservation reaction for 24h to obtain the reaction solution.

[0040] (2) Pour the reaction solution into a separatory funnel and carry out static layering treatment for 0.5h, then take the upper layer to obtain the upper layer A.

[0041] (3) Add an aqueous oxalic acid solution with a mass concentration of 2% to the supernatant liquid A for stratification, and take the upper layer to obtain a supernatant liquid B; wherein, the molar mass of oxalic acid in the oxalic acid aqueous solution is 3 mol.

[0042] (4) After adding 3mol sherwood oil and saturated sodium bicarbonate...

technical field

[0001] The invention belongs to the field of chemical synthesis, in particular to a synthetic method of vitamin B6 triisopalmitate. Background technique

[0002] Vitamin B6 triisopalmitate is a common pharmaceutical intermediate and industrial raw material, which is generally synthesized from vitamin B6 (Vitamin B6).

[0003] However, the traditional synthetic method of vitamin B6 triisopalmitate is relatively complicated, and the price of the raw materials used is unstable, and it is easy to produce more waste gas, waste water and waste residue, which is not good for the environment. Therefore, it is urgent to study a low-cost A cost-effective and environmentally friendly synthesis method of vitamin B6 triisopalmitate. Contents of the invention

[0004] The purpose of the embodiments of the present invention is to provide a synthetic method of vitamin B6 triisopalmitate, aiming to solve the problems raised in the background technology.

[0005] The embod...

Examples

Embodiment 1

[0024] This embodiment provides a kind of synthetic method of vitamin B6 triisopalmitate, it comprises the following steps:

[0025] (1) 1mol of vitamin B6 hydrochloride, 5mol of pyridine and 7mol of cyclohexane were mixed for 30min, and placed in an ice bath at a temperature of 15°C, then 2mol of 2-hexyldecanoyl chloride was added dropwise ( Control the dropwise addition within 4h) to carry out the heat preservation reaction for 24h to obtain the reaction solution.

[0026] (2) Pour the reaction solution into a separatory funnel and carry out static layering treatment for 0.1h, then take the upper layer to obtain the upper layer A.

[0027] (3) Add an aqueous oxalic acid solution with a mass concentration of 1% to the supernatant A for stratification, and take the upper layer to obtain a supernatant B; wherein, the molar mass of oxalic acid in the oxalic acid aqueous solution is 2 mol.

[0028] (4) After adding 2mol sherwood oil and saturated sodium bicarbonate solution to l...

Embodiment 2

[0031] This embodiment provides a kind of synthetic method of vitamin B6 triisopalmitate, it comprises the following steps:

[0032] (1) 1mol of vitamin B6 hydrochloride, 7mol of pyridine and 9mol of cyclohexane were mixed for 30min, and placed in an ice bath at a temperature of 5° C., then added dropwise with 4mol of 2-hexyldecanoyl chloride ( Control the dropwise addition within 4h) to carry out the heat preservation reaction for 24h to obtain the reaction solution.

[0033] (2) Pour the reaction solution into a separatory funnel for static layering treatment for 1 h, then take the upper layer to obtain the upper layer A.

[0034] (3) Add an aqueous oxalic acid solution with a mass concentration of 3% to the supernatant A for stratification, and take the upper layer to obtain a supernatant B; wherein, the molar mass of oxalic acid in the oxalic acid aqueous solution is 4mol.

[0035] (4) After adding 4mol sherwood oil and saturated sodium bicarbonate solution to layering in...

Embodiment 3

[0038] This embodiment provides a kind of synthetic method of vitamin B6 triisopalmitate, it comprises the following steps:

[0039] (1) 1mol of vitamin B6 hydrochloride, 6mol of pyridine and 8mol of cyclohexane were mixed for 30min, and placed in an ice bath at a temperature of 10°C, then 3mol of 2-hexyldecanoyl chloride was added dropwise ( Control the dropwise addition within 4h) to carry out the heat preservation reaction for 24h to obtain the reaction solution.

[0040] (2) Pour the reaction solution into a separatory funnel and carry out static layering treatment for 0.5h, then take the upper layer to obtain the upper layer A.

[0041] (3) Add an aqueous oxalic acid solution with a mass concentration of 2% to the supernatant liquid A for stratification, and take the upper layer to obtain a supernatant liquid B; wherein, the molar mass of oxalic acid in the oxalic acid aqueous solution is 3 mol.

[0042] (4) After adding 3mol sherwood oil and saturated sodium bicarbonate...