Structure of 1046806-03-4
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The BI-3802 was designed by Boehringer Ingelheim and could be obtained free of charge through the Boehringer Ingelheim open innovation portal opnMe.com, associated with its negative control.
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Search for reports by entering the product batch number.
Batch number can be found on the product's label following the word 'Batch'.
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Batch number can be found on the product's label following the word 'Batch'.
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CAS No. : | 1046806-03-4 |
Formula : | C27H31BrN6O3 |
M.W : | 567.48 |
SMILES Code : | CC(N1C(CNC2=CC=C(C#N)C=C2)N(C)C3(CC)C1=CC(N(C4=NC=CC=C4)C=O)=CC3)C(O)=O.[H]Br |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen bromide; In water; isopropyl alcohol; at 7 - 38℃; for 1.33333h;pH 0.6 - 1.3;Industry scale; | Example 1 - Large-scale industrial synthesis of the compound of formula 4-Br88 kg carbonyl-di-(l,2,4-triazole) are taken and combined with 920 1 tetrahydrofuran. The contents of the apparatus are heated to 35C with stirring. Then 90 kg of compound 3 are added batchwise at 35C within 1 to 2 hours.160 kg of compound 2 are placed in a second reaction vessel, then 350 1 tetrahydrofuran are added and the mixture is heated to 500C with stirring.The solution of 3 is metered into the solution of 2 within 2 to 3 hours at 47C - 53C and the solution obtained is diluted with 115 1 tetrahydrofuran. Then the mixture is stirred for another 4 hours at 47C - 53C ( preferably 500C ). Then 670 1- 695 1 tetrahydrofuran are distilled off in vacuo at 50C-60C. 235 1 of n-butyl acetate are then allowed to flow into the residue. After this, 600 1 -630 1 of a butyl acetate/THF mixture are distilled off in vacuo at 50C-85C. During the distillation 700 1 butyl acetate are metered in. 65 kg acetic acid are allowed to flow into the residue, the contents are heated to 85C-90C and stirred for at least another 2.5 h at this temperature. Then the mixture is cooled to 65C-75C. A solution of 165 1 water and 20 kg common salt is added to the contents and the mixture is rinsed with 300 1 water. Then the temperature is adjusted to 60C-70C and the mixture is stirred for a minimum of 15 min. at this temperature. For phase separation the stirrer is stopped and the mixture is left to settle for at least 15 min. The aqueous phase is drained off into another reaction vessel which contains 120 1 of n-butyl acetate. The mixture is heated to 60C-70C with stirring and stirred for at least 10 min. After phase separation the aqueous phase is drained off into the chemical waste drain. The butyl acetate phases and 20 1 of butyl acetate for rinsing are combined. 590 1 - 620 1 of n-butyl acetate are distilled off from this content in vacuo at a max. internal temperature of 800C. <n="12"/>880 1 isopropanol are allowed to flow into the distillation residue and the content is adjusted to 32C-38C. Then approx. 90 kg of 48% hydrobromic acid are metered in at 32C-38C until the pH value is 0.6 to 1.3. The mixture is stirred for a minimum of 20 min. at 32C-38C and then cooled to 7C-13C and stirred at this temperature for at least one hour. The resulting suspension is centrifuged, washed with a total of 840 1 isopropanol and dried in vacuo at max. 55C. Yield: 211 kg-250 kg. Mp.: 200-2150C (with decomposition). |
Tags: 1046806-03-4 synthesis path| 1046806-03-4 SDS| 1046806-03-4 COA| 1046806-03-4 purity| 1046806-03-4 application| 1046806-03-4 NMR| 1046806-03-4 COA| 1046806-03-4 structure
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