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CAS No. : | 72648-12-5 | MDL No. : | MFCD00160150 |
Formula : | C6H3Cl4N | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | TZKVGCQBQQFWOV-UHFFFAOYSA-N |
M.W : | 230.91 | Pubchem ID : | 606698 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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* 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 chlorine;pelletized catalyst TOSOH HSZ-690 HOD (SAR 203) with a silica binder; at 350℃;Gas phase;Product distribution / selectivity; | Example 2; The pelletized catalyst, TOSOH HSZ-690 HOD (SAR 203) with a silica binder, was ground to a coarse powder and screened to obtain a uniform size of 1-2 mm in diameter. A weight of 0.26 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. Operating at a chlorine feed of 5 cc/min, a beta-picoline feed rate of 0.13 mg/min (10 cc/min N2 with a chiller temperature of 10 C.), the reagents were fed to the reactor at an initial temperature of 250 C. The system was initially ramped up to 325 C. and allowed to stablize. Under these conditions the product gases were 18.5% 3-trichloromethylpyridine (beta-tri ) and 65.4% beta-2-tet. When the system was allowed to stabilized at 350 C. the amount of beta-tri in the product gases was reduced to 2.6% and the conversion to beta-2-tet increased to 68.6% (see Table 2).; Example 3; The catalyst, TOSOH HSZ-690 HOD (SAR 203) with the silica binder, was sized to a uniform particle size of 1-2 mm in diameter. A weight of 0.26 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. The reactor temperature was initially set to 250 C. prior to flowing chlorine at a rate of 5 cc/min. The beta-picoline feed rate was set to 0.13 mg/min (N2 flow 10 cc/min, chiller at 10 C.), while the reactor oven was ramped up to 350 C. over a one hour time period. At 350 C. the amount of beta-2-tet observed in the product gases was 65.6% (see Table 2).; Example 4; The catalyst, TOSOH HSZ-690 HOD (SAR 203) with the silica binder, was sized to a uniform particle size of 1-2 mm in diameter. A weight of 0.51 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. The reactor temperature was initially set to 250 C. prior to flowing chlorine at a rate of 5 cc/min. The beta-picoline feed rate was set to 0.13 mg/min (chiller at 10 C.), with a nitrogen flow of 10 cc/min, while the reactor oven was ramped up to 350 C. over 2 hours. When the system had stabilized at 350 C. the amount of beta-2-tet observed in the product gases was 71.7% (see Table 2).; Example 5; The catalyst, TOSOH HSZ-690 HOD (SAR 203) with the silica binder, was sized to a uniform particle size of 1-2 mm. A weight of 0.51 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. The reactor temperature was initially set to 250 C. prior to flowing chlorine at a rate of 5 cc/min. The beta-picoline feed rate was set to 0.25 mg/min (N2 at 10 cc/min, chiller at 20 C.), while the reactor oven was slowly ramped up to 350 C. over 2 hours. When the system had stabilized at 350 C. the amount of beta-2-tet observed in the product gases was 66.9% (see Table 2). | |
With chlorine; at 400℃;Gas phase;Product distribution / selectivity; | Example A; This is the control run where the reactor contained glass wool (Pyrex) plugs and no catalyst. The reactor temperature was initially set to 350 C. prior to feeding chlorine at a rate of 5 cc/min. The beta-picoline feed rate was set to 0.25 mg/min (N2 at 10 cc/min, chiller at 20 C.) at the oven temperature of 350 C. When the system had stabilized the amount of beta-2-tet was only 8.7%, with the majority of the conversion going to beta-tri (65.4%). When the temperature was increased to 400 C. the amount of beta-2-tet increased to 46.1% with a reduction in beta-tri (21.5%). A fair amount of over chlorinated 2,6-dichloro-3-trichloromethylpyridine (beta-2,6-penta,12.2%) was also observed (see Table 2). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
47%Chromat.; 21%; 4.8%Chromat.; 11%Chromat. | With tetrachloromethane; at 200 - 350℃; for 0.00305556h;Molecular sieve; Inert atmosphere; | 40 G ZSM - 5 molecular sieve (silicon-aluminum ratio 200, strip (1 - 2 mm)) by adding [...] 60 cm, diameter of 2.4 cm cylindrical quartz tube, the upper end of the catalyst filling 10 g of inert ceramic ball (diameter 4 mm), the quartz tube using the resistance wire heating. The constant pressure in the funnel 8 g 3 - methyl pyridine and 70 g CCl4[...] 200 C flask, 2 h the raw materials of the completion of the dropping, of the 3 - methyl pyridine with CCl4The steam is N2The carrier gas to the quartz tube, N2The flow rate control in 250 ml/min. Cl2In order to 300 ml/min flow rate individually to the quartz tube with the raw material of the steam in the catalyst bed on the reaction, the reaction temperature is 350 C, time is 11 s. The reaction mixture through the receiving flask condensation, GC normalized 3 - methyl pyridine totally transformed, 3 - dichloro pyridine and isomer 47%, 2 - chloro -5 - trichloromethyl pyridine 27%, 2 - chloro -3 - trichloromethyl pyridine 4.8%, 2, 3 - dichloro -5 - trichloromethyl pyridine 11%. The purity of the purification after rectification>99% of 2 - chloro -5 - trichloromethyl pyridine, the yield of 21%. |
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