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. 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, A new synthetic method of this compound is introduced below., Recommanded Product: 2062-98-8
To a 3 -neck flask equipped with a temperature probe, magnetic stir bar, water- cooled condenser, and addition funnel was charged sodium borohydride (16.0 g, 423 mmol), and tetraethylene glycol dimethyl ether (125 mL). 2,3,3,3-Tetrafluoro-2- (1,1,2,2,3, 3, 3-heptafluoropropoxy)propanoyl fluoride (100 g, 301 mmol) was added dropwise to the resultant mixture. After complete addition, the reaction mixture was heated to reflux and stirred overnight. The mixture was then allowed to cool to room temperature followed by the dropwise addition of methanol (100 mL) and H2O (150 mL). The mixture was then transferred to a separatory funnel and the fluorous phase was collected and then distilled (46.1 C, 40 ton) to afford 2,3,3,3-tetrafluoro-2-(l, 1,2,2,3,3- heptafluoropropoxy)propan-l-ol (67.5 g, 71%) as a colorless liquid. The isolated compound was used in the next step. (0204) To a 3-neck flask equipped with a temperature probe, distillation head, overhead stirrer, and under N2 was charged TiCU (7.9 mL, 72 mmol). 2,3,3,3-Tetrafluoro-2- (l,l,2,2,3,3,3-heptafluoropropoxy)propan-l-ol (15.1 g, 47.8 mmol) was added dropwise with stirring and the resultant mixture was heated to 40 C followed by a 30 min stir. The mixture was then allowed to cool to room temperature followed by the dropwise addition of tetraethylene glycol dimethyl ether (45 mL). Exotherms reaching approximately 50 C were observed. The resultant mixture was allowed to warm to room temperature followed by the addition of zinc dust (9.1 g, 140 mmol) in one portion. The resultant reaction mixture was raised to 85 C. After a 3 h stir, the temperature was slowly raised to 225 C and distillate was collected with the distillation head temperature reaching 69 C affording the title compound (4.1 g, 31%) as a colorless liquid.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; 3M INNOVATIVE PROPERTIES COMPANY; SMITH, Sean M.; LAMANNA, William M.; COSTELLO, Michael G.; BULINSKI, Michael J.; (35 pag.)WO2017/195070; (2017); A1;,
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