Method for pipelined synthesis of vitamin H intermediate
A synthesis method and compound technology, applied in the field of medicine, can solve the problems of low conversion rate, large amount of triphosgene, etc., and low safety
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[0064] The first aspect of the present invention provides a synthetic method for a compound of formula 3, comprising the steps of:
[0065]
[0066] (1) Salt solution, triphosgene (BTC) solution and potassium hydroxide solution of compound of formula 2 are provided;
[0067] (2) The salt solution of the compound of formula 2, triphosgene (BTC) solution and potassium hydroxide solution are mixed, and the resulting mixed solution is continuously fed into the pipeline reactor for reaction; and
[0068] (3) adjusting the pH of the reacted reaction solution to acidity to obtain the compound of formula 3;
[0069] Wherein, the salt is the potassium salt and / or sodium salt of the compound of formula 2.
[0070] In another preferred embodiment, the mixing of the feed in step (2) is feeding while mixing.
[0071] In another preference, step (2) also includes steps before:
[0072] Pre-cool the salt solution of the compound of formula 2, triphosgene (BTC) solution and potassium hy...
Embodiment 1
[0105] 37.2g (0.100mol) of the formula 2 compound disodium salt was dissolved in 200g of water (mass concentration 14.9%) to obtain solution A; 19.3g (0.065mol) of triphosgene (two (trichloromethyl) carbonate) Dissolve in 77.0 g of toluene (mass concentration 20%) to obtain solution B; solution C is an aqueous potassium hydroxide solution with a mass concentration of 25%. Pre-cool the three solutions of A, B, and C to 10-15°C, then mix them in the mixer according to the mass ratio of A:B:C=3.83:1.57:1, and send them to the pipeline reactor through a peristaltic pump. (Tube length 10 meters, pipe diameter 10 millimeters) feeding, start reaction, control reaction temperature at 10~30 ℃ in the reaction process. Fine-tune the feed rate of solution C according to the pH value of the sampling in the middle of the pipeline reactor, control the pH of the sample to be 8-9, and the residence time of the mixed solution in the pipeline reactor is about 15 minutes. After the reaction is c...
Embodiment 2
[0107] The disodium salt of formula 2 compound of 37.2g (0.100mol) is dissolved in the water (mass concentration 14.9%) of 200g to obtain solution A; The triphosgene of 20.7g (0.070mol) is dissolved in the toluene of 83.0g (mass concentration 20%) %) obtains solution B; Solution C is the potassium hydroxide aqueous solution of mass concentration 25%. Pre-cool the three solutions of A, B, and C to 10-15°C, then mix them in the mixer according to the mass ratio of A:B:C=3.80:1.65:1, and send them to the pipeline reactor through a peristaltic pump. (The length of the tube is 10 meters, and the tube diameter is 10 mm). Feed slowly to start the reaction. During the reaction, the reaction temperature is controlled at 10-30°C. Fine-tune the feed rate of solution C according to the pH value of the sampling in the middle of the pipeline reactor, control the pH of the sample to be 8-9, and the residence time of the mixed solution in the pipeline reactor is about 15 minutes. The reactio...
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