Compound manufacturing method
A manufacturing method and compound technology, which is applied in the preparation of organic compounds, hydrocarbons, hydrocarbons, etc., can solve the problems of undocumented organic base manufacturing methods, and achieve the effect of excellent and high reaction speed
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[0531] Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited to these Examples.
[0532]
[0533] Measuring device: CBM-20A (manufactured by Shimadzu Corporation)
[0534] Column: L-Column2 ODS (3μm, 4.6mmφ×25cm)
[0535] Mobile Phase A: Acetonitrile
[0536] Mobile phase B: THF
[0537] Mobile phase C: pure water
[0538] Gradient: 0.01 minutes A=60%, B=0%, C=40%
[0539] 10 minutes A=60%, B=0%, C=40%
[0540] 20 minutes A=100%, B=0%, C=0%
[0541] 100 minutes A=100%, B=0%, C=0%
[0542] 120 minutes A=0%, B=100%, C=0%
[0543] 130 minutes A=0%, B=100%, C=0%
[0544] Flow: 1.0mL / min
[0545] Detection wavelength: 280nm.
[0546]
[0547] Measuring device: HLC-822GPC (manufactured by Tosoh Corporation)
[0548] Column: PLgel 10 μm MIXED-B (manufactured by Tosoh Corporation)
[0549] Column temperature: 40°C
[0550] Mobile phase: tetrahydrofuran
[0551] Flow rate: 1.5mL / min
[0552] Detection wavelength: 228nm....
Embodiment 1
[0571] Synthesis of compound (5-1)
[0572] Compound (1-1) was synthesized according to the method described in International Publication No. 2002 / 045184.
[0573] For the compound (2-1), 4-biphenylboronic acid manufactured by Tokyo Chemical Industry Co., Ltd. was used.
[0574] After the reaction vessel was made into a nitrogen gas atmosphere, compound (1-1) (1.93g), compound (2-1) (2.43g), phenanthrene (0.316g) (internal standard substance), dichlorobis[tris (2-Methoxyphenyl)phosphine]palladium (1.18mg), toluene (100g) and pinacol (0.26g), heated to 86°C. Then, 20% tetraethylammonium hydroxide aqueous solution (15g) was added there, and it stirred at 86 degreeC for 2 hours. As a result of LC analysis of the obtained reaction mixture, the internal standard yield of the target compound (5-1) was 99%. The results are shown in Table 1.
[0575] [Table 1]
[0576] .
[0577] From the comparison of the yield of compound (5-1) in Comparative Example 1 and the yield of comp...
Synthetic example 1
[0578] Synthesis of Polymer Organic Compound P-1
[0579] [chemical formula 81]
[0580]
[0581] (In the formula, n represents the degree of polymerization).
[0582] Compound (1-2) was synthesized according to the method described in International Publication No. 2002 / 045184.
[0583] Compound (2-2) was synthesized according to the method described in US Patent No. 6,169,163.
[0584] After making the reaction vessel into a nitrogen gas atmosphere, compound (1-2) (7.22 g), compound (2-2) (9.90 g), dichlorobis[tris(2-methoxyphenyl)phosphine] were added Palladium (4.15 mg) and toluene (131 g), heated to 86°C. Then, 10% tetramethylammonium hydroxide aqueous solution (108g) and tetrabutylammonium bromide (0.51g) were added there, and it stirred at 86 degreeC for 2 hours. After cooling the obtained reaction mixture to room temperature, toluene (1096g) was added and diluted and liquid-separated, and water (324g) was added and liquid-separated. After dripping the obtained ...
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