Preparation method of dimethyl L-dibenzoyl tartarate
A technology of benzoyl dimethyl tartrate and benzoyl tartaric acid is applied in the field of preparation of L-dibenzoyl tartrate, and can solve the problems that by-products and products are not easily separated, the yield of target products is low, and the variety of raw materials There are many problems such as avoiding the production of by-product benzoic acid, the color of the product is pure white, and the conversion rate is improved.
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Embodiment 1
[0025] A kind of preparation method of L-dibenzoyl tartrate dimethyl that the present invention proposes comprises the following steps:
[0026] Preparation of S1, L-dibenzoyl tartaric anhydride:
[0027] a. Add toluene, L-tartaric acid and Lewis acid into the reaction kettle, heat up to 85°C while stirring, cool down to 75°C after stirring and mixing evenly, and then slowly add benzoyl chloride and thionyl chloride dropwise, controlled at 4h After the internal addition is completed, keep warm for 2 hours, follow the reaction by TLC, cool down to 30°C after the reaction is completed, and centrifuge to obtain the crude product of L-dibenzoyl tartaric anhydride, wherein the Lewis acid is ferric chloride, L-tartaric acid, benzoyl tartaric anhydride The mol ratio of acid chloride and thionyl chloride is 1:2:1.1; the mass ratio of L-tartaric acid and toluene is 1:1.6; the mass ratio of L-tartaric acid and Lewis acid is 1:0.0008;
[0028] b. Put the crude product of L-dibenzoyl tar...
Embodiment 2
[0035] A kind of preparation method of L-dibenzoyl tartrate dimethyl that the present invention proposes comprises the following steps:
[0036] Preparation of S1, L-dibenzoyl tartaric anhydride:
[0037] a. Add toluene, L-tartaric acid and Lewis acid into the reaction kettle, heat up to 88°C while stirring, cool down to 78°C after stirring and mixing evenly, and then slowly add benzoyl chloride and thionyl chloride dropwise, controlled at 4h The internal addition was completed, and the temperature was kept for 2 hours. TLC followed the reaction. After the reaction was completed, the temperature was lowered to 33°C, and the crude product of L-dibenzoyl tartaric anhydride was obtained by centrifugal separation. Among them, the Lewis acid was aluminum trichloride, L-tartaric acid, benzoyl The mol ratio of acid chloride and thionyl chloride is 1:2.02:1.1; the mass ratio of L-tartaric acid and toluene is 1:1.8; the mass ratio of L-tartaric acid and Lewis acid is 1:0.0009;
[0038...
Embodiment 3
[0045] A kind of preparation method of L-dibenzoyl tartrate dimethyl that the present invention proposes comprises the following steps:
[0046] Preparation of S1, L-dibenzoyl tartaric anhydride:
[0047] a. Add toluene, L-tartaric acid and Lewis acid into the reaction kettle, heat up to 90°C while stirring, cool down to 80°C after stirring and mixing evenly, and then slowly add benzoyl chloride and thionyl chloride dropwise, controlled at 4h After the internal addition was completed, the temperature was kept for 2 hours, and the reaction was tracked by TLC. After the reaction was completed, the temperature was lowered to 35°C, and the crude product of L-dibenzoyl tartaric anhydride was obtained by centrifugal separation. Among them, the Lewis acid was zinc chloride, L-tartaric acid, and benzoyl chloride The mol ratio with thionyl chloride is 1:2.05:1.1; The mass ratio of L-tartaric acid and toluene is 1:2; The mass ratio of L-tartaric acid and Lewis acid is 1:0.001;
[0048]...
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