|Unit Price:||USD 1.0000 / Kilogram |
|Min. Order:||1 Kilogram|
|Delivery Time:||15 Days|
Model No.: 5807-14-7
Packaging: AS REQUIRED
Place of Origin: CHINA
Supply Ability: TRUE MANUFACTURER
1,3,4,6,7,8-Hexahydro-2H-pyrimido[1,2-A]pyrimidine CAS number is 5807-14-7, commonly known as bicyclic guanidine, abbreviated as TBD. He is an organic strong base that exhibits good catalytic effects on various organic reactions and polymerization reactions. Regarding his synthesis, a method for synthesizing TBD using bis(3-aminopropyl)amine and hydrazine hydrochloride as a raw material in the absence of a solvent has been reported in the literature. The problem with this method is that since the polarities of the two raw materials are so different that they are not mutually soluble, the hydrazine hydrochloride solids react with the bis(3-aminopropyl)amine liquid in a heterogeneous manner. The reaction time is Longer, more side reactions, less product purity, and difficult separation. Finding a suitable amphiphilic reaction solvent system to make the two reactants react under homogeneous conditions is one of the effective ways to increase the yield and purity of TBD.
There is an improved method we think is more feasible, probably the process is as follows:
(1) The bis (3-aminopropyl) amine and hydrazine hydrochloride were dissolved in a hydrophobic solvent and a hydrophilic solvent, respectively, to control the concentration of each solution At 1.0-10.0 mol/L, the molar ratio of hydrazine hydrochloride to bis(3-aminopropyl)amine was controlled to be 1:1. The above hydrophobic solvent is specifically mesitylene or mesitylene, and the hydrophilic solvent is specifically diethylene glycol or triethylene glycol.
(2) adding the above bis(3-aminopropyl)amine solution to a reaction vessel equipped with a reflux condenser and a stirring device, followed by the addition of a hydrazine hydrochloride molar amount of 0.001% to 0.005% TBD as a catalyst;
(3) Under argon protection, maintain the reaction temperature at 120-145°C, add the hydrazine hydrochloride solution prepared in step (1) dropwise into the reactor, and control the addition within 0.5-1.0h. After the completion of the reaction to 3.0-4.5h;
(4) After the reaction is complete, spin-dry the biparental mixed solvent to obtain a white solid, namely TBD hydrochloride;
(5) After dissolving the hydrochloride of TBD with water, adding sodium hydroxide to adjust the aqueous solution to pH 10-12, and adding dichloromethane to extract, the obtained methylene chloride solution is TBD dichloromethane solution;
(6) The obtained TBD dichloromethane solution was obtained by spin-drying the methylene chloride to obtain a white or slightly yellow solid which was vacuum dried for 24 to 48 hours, to obtain the product TBD, the yield was ≥95.0% and the purity was ≥98.0%.
This method is simple in operation, high in yield of the target product, and high in product purity.
Thera. Category: Muscle Relaxant
Cas No.: 5807-14-7
Synonym:TBD;2H-Pyrimido[1,2-a]pyrimidine, 1,3,4,6,7,8-hexahydro-;1,5,7-Triazabicylo[4.4.0]dec-5-ene;Silicagel, functionalized, 1,5,7-Triazabicyclo[4,4,0]dec-5-ene, 1.4;LABOTEST-BB LT00847641;1,5,7-TRIAZABICYCLO[4.4.0]DEC-5-ENE;1,3,4,6,7,8-HEXAHYDRO-2H-PYRIMIDO[1,2-A]PYRIMIDINE;1,3,4,6,7,8-HEXAHYDRO-2H-PYRIMIDO[1,2-A]PYRIMIDINE, POLYMER-BOUND;
Molecular Weight: 139.2
Molecular formulate: C7H13N3
Appearance: White Crystalline solid
Packing:Export worthy packing
Material Safety Data Sheet:Available on request