Synthesis method of D-para-methoxy dibenzoyl tartaric acid
A technology of methoxydibenzoyl tartaric acid and methoxybenzoyl chloride, which is applied in the direction of organic chemical methods, chemical instruments and methods, and carboxylate preparation, and can solve the problems of large pollutant generation, long synthesis steps, Problems such as high production cost, to achieve the effect of wide application range, convenient post-processing, and product cost reduction
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Embodiment 1
[0021] A kind of synthetic method of D-p-methoxydibenzoyl tartaric acid proposed by the present invention comprises the following steps:
[0022] Preparation of S1, D-p-methoxydibenzoyl tartaric anhydride:
[0023] Add p-methoxybenzoyl chloride and xylene to the reaction kettle, raise the temperature to 130°C, then slowly add D-tartaric acid, keep warm for 1 hour after the addition is complete, follow the reaction with TLC, cool down to 25°C after the reaction, keep warm for 1 hour to crystallize, Then add methanol to the reaction kettle, stir for 0.5h, then centrifuge to dry, rinse the filter cake with a small amount of water, and purify to obtain the wet product of D-p-methoxydibenzoyl tartaric anhydride; the D-tartaric acid and p-methoxy The molar ratio of benzoyl chloride is 1:3.0; the mass ratio of D-tartaric acid and xylene is 1:1.2;
[0024] Preparation of S2, D-p-methoxydibenzoyl tartaric acid:
[0025] a. Add pure water and D-p-methoxydibenzoyl tartaric anhydride we...
Embodiment 2
[0028] A kind of synthetic method of D-p-methoxydibenzoyl tartaric acid proposed by the present invention comprises the following steps:
[0029] Preparation of S1, D-p-methoxydibenzoyl tartaric anhydride:
[0030] Add p-methoxybenzoyl chloride and xylene into the reaction kettle, raise the temperature to 133°C, then slowly add D-tartaric acid, keep warm for 3 hours after the addition is complete, TLC to follow the reaction, after the reaction is completed, cool down to 28°C, keep warm for 1 hour to crystallize, Then add methanol to the reaction kettle, stir for 0.5h, then centrifuge to dry, rinse the filter cake with a small amount of water, and purify to obtain the wet product of D-p-methoxydibenzoyl tartaric anhydride; the D-tartaric acid and p-methoxy The mol ratio of benzoyl chloride is 1:3.05; the mass ratio of D-tartaric acid and xylene is 1:1.6;
[0031] Preparation of S2, D-p-methoxydibenzoyl tartaric acid:
[0032] a. Add pure water and D-p-methoxydibenzoyl tartari...
Embodiment 3
[0035] A kind of synthetic method of D-p-methoxydibenzoyl tartaric acid proposed by the present invention comprises the following steps:
[0036] Preparation of S1, D-p-methoxydibenzoyl tartaric anhydride:
[0037] Add p-methoxybenzoyl chloride and xylene into the reaction kettle, raise the temperature to 135°C, then slowly add D-tartaric acid, keep warm for 5 hours after the addition is complete, TLC to follow the reaction, after the reaction is completed, cool down to 30°C, keep warm for 1 hour to crystallize, Then add methanol to the reaction kettle, stir for 0.5h, then centrifuge to dry, rinse the filter cake with a small amount of water, and purify to obtain the wet product of D-p-methoxydibenzoyl tartaric anhydride; the D-tartaric acid and p-methoxy The molar ratio of benzoyl chloride is 1:3.1; the mass ratio of D-tartaric acid and xylene is 1:2;
[0038] Preparation of S2, D-p-methoxydibenzoyl tartaric acid:
[0039] a. Add pure water and D-p-methoxydibenzoyl tartaric...
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