Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 13401-56-4, name is 3-Chloro-2,2-dimethylpropan-1-ol. A new synthetic method of this compound is introduced below., name: 3-Chloro-2,2-dimethylpropan-1-ol
2. Preparation of 3-Chloro-2,2-dimethyl-1-trimethylsilyloxy-propane at 100 C., Lot 9279 A 500 milliliter, three-necked flask was fitted with a large magnetic stir bar, a reflux condenser, a thermocouple attached to a THERM-O-WATCH, a 125 ml. pressure-equalizing addition funnel, and an argon inlet. This apparatus was dried in an oven overnight at 125 C., assembled hot, and allowed to cool to room temperature in a stream of argon. The flask was charged with 122.68 grams (1.00 mole, 1.00 equivalent) of 3-chloro-2,2-dimethyl-1-propanol. Hexamethyldisilazane, 83.35 grams (0.516 mole, 0.516 equivalent), was then added dropwise via the addition funnel. Trimethylsilylchloride catalyst, one ml., was added via a syringe. An immediate exotherm of 23.4 C. was observed. A white precipitate also formed when the catalyst was added. The reaction mixture was heated to 100 C. with a heating mantle, controlled by the THERM-O-WATCH. Periodically, an aliquot was removed, filtered through a 0.45 micron syringe filter, and analyzed by Gas Chromatography (GC), thirty meter*0.53 mm AT-1 column. After twenty-four hours at 100 C., both of the starting materials were still present. Therefore, an additional 0.5 ml. of trimethylsilylchloride was added. After forty-eight hours at 100 C., both of the starting materials were still present. Therefore, an additional 0.5 ml. of trimethylsilylchloride was added. After a total of seventy-two hours at 100 C., all the starting 3-chloro-2,2-dimethyl-1-propanol had been consumed, with the formation of a single, higher-boiling component. The heat source was removed. After the reaction mixture had cooled to room temperature, it was transferred to a medium porosity sintered glass filter. The filtrate was collected in a dry 250 ml. bottle. This afforded a clear, very pale yellow solution, yield=178.37 grams (91.65% yield).
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Reference:
Patent; FMC Corporation; US5543540; (1996); A;,
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