Adding a certain compound to certain chemical reactions, such as: 53145-38-3, name is 2-Chloro-6-fluoroanisole, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 53145-38-3, Formula: C7H6ClFO
The system 100 shown in FIG. 1 was configured with a first reactor 102 having an internal volume of about 25 ml, a transfer tube 106 having an internal volume of about 3 ml and a second reactor 104 having an internal volume of about 30 ml.Agitation was started in the first reactor 102 and the second reactor 104. The system 100 was cooled to about -60 C. by placing the first reactor 102 and the second reactor 104 in the bath 108 containing dry ice in hexane and maintained at a temperature of about -70 C. A solvent level of the bath 108 was checked to assure that the transfer tube 106 was covered with the solvent.A solution of 2-chloro-6-fluoroanisole (2,6-CFA) (31.4 g, 190 mmol) in anhydrous 1,2-dimethoxyethane (DME) (241 ml) was prepared in a 500 ml bottle. Molecular sieves were added to remove water, and water content was measured by Karl Fischer titration to assure the 2,6-CFA solution contained less than about 100 ppm water (about 35 ppm measured). The 2,6-CFA solution in the 500 ml bottle was placed on a balance and fitted with a cap holding the inlet tube to metering pump 110. (i.e, first pump 110). A mixture of n-butyllithium in hexanes (2.5 M, 102 ml) was loaded into another (syringe) pump (i.e., second pump 112) and trimethyl borate (25.7 g, 28 ml) was loaded into a syringe and was placed on a separate syringe pump (i.e., third pump 114).The first, second, and third feed lines 118, 120, 122 were respectively pumped full of the 2,6-CFA, the n-butyllithium and the methyl borate to just short of the tube exit prior to the start of the experiment. When the solvent bath temperature was about -74 C., the first pump 110 containing the 2,6-CFA and the second pump 112 containing the n-butyllithium were started with flow rates of 0.73 ml/min and 0.27 ml/min, respectively. The first feed line 118 was formed from polytetrafluoroethylene (PTFE) tubing and was directed through the reactor head port 116A into the first reactor 102 below the liquid surface. The n-butyllithium addition was added to the first reactor 102 through the second feed line 120 that terminated just above the liquid surface in the first reactor 102.The solvent bath was monitored and dry ice was added to the solvent bath to maintain the temperature of the system 100 at less than about -60 C. The third feed line 122 for the trimethyl borate was directed into the second reactor 104 to drip above the liquid surface. After about 26 minutes, when the first reactor 102 was full and the reaction mixture was flowing through the transfer tube into the second reactor 104, the third pump 114 was started at a flow rate of the trimethyl borate of about 0.08 ml/min.After about 37 minutes, as the second reactor 104 filled, flow was started from an exit tube 126 to maintain reaction mixture volume in the second reactor 104 near about 30 ml. Intermediate solution from the second reactor 104 was accumulated in the flask 124 at room temperature. The intermediate solution was weighed and transferred to sample jars every 20 to 30 minutes. The experiment was run for 4 hours. A total of about 153 g of the intermediate solution containing PBA-diMe was collected. A gas chromatography (GC) method with internal standard was used to quantify the amount of PBA-diMe in the intermediate solution. A conversion to PBA-diMe of about 92% was calculated with about 8% of the original unconverted 2,6-CFA also quantified.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Chloro-6-fluoroanisole, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; DOW AGROSCIENCES LLC; Emonds, Mark V. M.; Menning, Catherine A.; Blaylock, D. Wayne; US2013/66115; (2013); A1;,
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