Electric Literature of 2062-98-8, A common heterocyclic compound, 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, molecular formula is C6F12O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
EXAMPLE 2: Example for preparation of CF3CF2CF2OCF (CF3) CF2OCOCF (CF3) OCF2CF2CF3 (1b) (fluorination step)[0090] Compound (3b) (200.0 g) obtained in Example 1, was dissolved in CF3CF2CF2OCF(CF3)COF (hereinafter referred to as compound (4b), 1000.0 g). On the other hand, into a 3000 mL autoclave made of nickel, NaF powder (260.5 g) was. put, and compound (4b) (2000.0 g) was added, followed by stirring and cooling to -10 DEG C. After supplying nitrogen gas for 1 hour, fluorine gas diluted to 20% with nitrogen gas, was supplied at a flow rate of 22.59 L/hr for 1 hour, and while supplying it at the same flow rate, the above fractional solution was injected over a period of 60 hours. [0091] Then, while supplying fluorine gas diluted to 20% with nitrogen gas, while maintaining the above flow rate, 20 mL of a solution of compound (4b) in benzene (0.01 g/mL) was injected, the outlet valve of the autoclave was closed, and when the pressure became 0.12 MPa, the inlet valve of the autoclave was closed, followed by stirring for 1 hour. Further, such an operation was repeated 4 times during a period until the temperature rose from -10 DEG C to room temperature and thereafter 5 times at room temperature. During the period, benzene was supplied in a total of 1.800 g, and compound (4b) was injected in a total of 281.0 g. Thereafter, nitrogen gas was supplied for 2 hours, and the reaction mixture was taken out by decantation. The obtained crude liquid was concentrated by an evaporator, and the product was quantified by <19>F-NMR, whereby it contained CF3CF2CF2OCF (CF3) CF2OCOCF (CF3) OCF2CF2CF3 (compound (1b)) in a yield of 69%. A part of the crude liquid was taken and distilled under reduced pressure to obtain compound (1b) . The boiling point of compound (1b) was from 46 to 51 DEG C/5.2 kPa.; EXAMPLE 3: Example for preparation of compound (1b) by a continuous process[0092] Using compound (2b) (75.5 g, 0.640 mol) and compound (1b) obtained in Example 2 (213.1 g, 0.321 mol), the reaction was carried out in the same manner as in Example 1 to obtain compound (3b) (amount: 272.4 g, 0.634 mol). The yield of compound (3b) as quantified by <1>H-NMR, was 99%. Then, the compound (3b) was reacted with fluorine in the same manner as in Example 2 to obtain compound (1b) (amount: 294.0 g, 0.44 mol). The same operation was repeated to finally obtain 3000 g of compound (1b).
The synthetic route of 2062-98-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ASAHI GLASS COMPANY LTD.; EP1352892; (2003); A1;,
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