A kind of preparation method of dimethyl-beta-thiatin propionate
A technology of thiotin propionate and dimethyl, which is applied in the field of preparation of new food attractants, can solve the problems of high production cost, insufficient reactivity, and high price of halogenated propionic acid, and achieve favorable cost control and reaction selectivity Good results
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Embodiment 1
[0019] Embodiment 1: the preparation method of a kind of dimethyl-beta-thiatin propionate of this example, its steps are:
[0020] A. Preparation of 3-(methylsulfonyloxy)propionic acid (II):
[0021] Add 3-hydroxypropionic acid (90g, 1.0mol), sodium bicarbonate (171g) and toluene (900g) into the reactor, stir evenly, cool in an ice bath and cool down to 0-10°C, and then add formazan dropwise Sulfonyl chloride (126g, 1.10mol), keep the temperature of the mixture between 0-10°C during the dropwise addition, remove the ice bath after the dropwise addition, continue to stir and react for 6 hours, after the reaction is completed, adjust the pH with 5% dilute hydrochloric acid to 2. Separation, the organic phase was dried over anhydrous sodium sulfate, and the solvent toluene was distilled off under atmospheric pressure to obtain the crude product of 3-(methylsulfonyloxy)propionic acid (II), which can be directly used in the next reaction without further purification . It is 137....
Embodiment 2
[0026] Embodiment 2: the preparation method of a kind of dimethyl-beta-propionate thiotin of this example, other steps are identical with embodiment 1, just the 3-(methylsulfonyloxy group) propionate (II) of A step The preparation method is as follows:
[0027] Add 3-hydroxypropionic acid (90g, 1.0mol), sodium bicarbonate (162g) and toluene (450g) into the reactor, stir evenly, cool in an ice bath and cool down to 0-10°C, then add formazan dropwise Sulfonyl chloride (114.5g, 1.0mol), keep the temperature of the mixture between 0-10°C during the dropwise addition, remove the ice bath after the dropwise addition, continue stirring for 4 hours, after the reaction, adjust the pH with 5% dilute hydrochloric acid To 2, liquid separation, the organic phase was dried over anhydrous sodium sulfate, and the solvent toluene was distilled off under atmospheric pressure to obtain the crude product of 3-(methylsulfonyloxy)propionic acid (II), which can be directly used in the next step with...
Embodiment 3
[0028] Embodiment 3: the preparation method of a kind of dimethyl-beta-propionate thiotin of this example, other steps are identical with embodiment 1, just the 3-(methylsulfonyloxy group) propionate (II) of A step The preparation method is as follows:
[0029] Add 3-hydroxypropionic acid (90g, 1.0mol), sodium bicarbonate (167g) and toluene (700g) into the reactor, stir evenly, cool in an ice bath and cool down to 0-10°C, and then add formazan dropwise Sulfonyl chloride (120.2g, 1.05mol), keep the temperature of the mixture between 0-10°C during the dropwise addition, remove the ice bath after the dropwise addition, continue stirring for 5 hours, after the reaction, adjust the pH with 5% dilute hydrochloric acid To 2, liquid separation, the organic phase was dried over anhydrous sodium sulfate, and the solvent toluene was distilled off under atmospheric pressure to obtain the crude product of 3-(methylsulfonyloxy)propionic acid (II), which can be directly used in the next step...
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