A kind of compound, palladium compound, nickel compound and preparation method thereof
A palladium compound, compound technology, applied in the direction of palladium organic compounds, nickel organic compounds, platinum group organic compounds, etc., can solve the problems of low activity, low copolymer molecular weight, low insertion ratio, etc., and achieve high activity, high copolymer molecular weight , the effect of high insertion ratio
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[0060] The present invention provides a kind of preparation method of the compound of formula (I) structure, comprising:
[0061] The compound of formula (II) structure reacts with the compound of formula (III) structure to obtain the compound of formula (IV) structure;
[0062] The compound of formula (IV) structure reacts with the compound of formula (V) structure, obtains the compound of formula (I) structure;
[0063]
[0064] Among them, R 1 One or more selected from H, C1-C6 alkoxy, substituted C1-C6 alkyl, C1-C6 alkyl, dimethylamino, nitro, halogen; the substitution of the substituted alkyl The group is fluorine;
[0065] R 2 , R 3 Independently selected from substituted phenyl or substituted biphenyl; the substituent of the substituted phenyl is selected from one or more of C1-C6 alkoxy and C1-C10 alkyl; the substituted biphenyl The substituent of the group is selected from one or more of C1-C6 alkoxy groups and C1-C10 alkyl groups;
[0066] R 4 It is selecte...
Embodiment 1
[0134] Example 1 Preparation of N-((2-methoxyphenyl)-12-phosphoryl)-N, P, P-triphenylphosphinamide
[0135]
[0136] At -78°C, dissolve aniline (0.9g, 10.0mmol) in 100ml EtO 2 Slowly add an equivalent to the solution n BuLi (2.5M in hexane, 4.4mL, 1.1eq) was stirred for 15min, reacted at room temperature for 1-2h, and added an equivalent of compound Ph to it at -78°C 2 POCl (2.4g, 10.0mmol), reacted at room temperature for 12h, and separated by column chromatography to obtain the target product A (where A does not need to be characterized, it can be directly used as a raw material for the next step). At 0°C, to dissolve A (2.925g, 10mmol) in 100ml THF solution, addn BuLi (2.5M in hexane, 4.4mL, 1.1eq) was reacted overnight at room temperature, compound B (3.08g, 1eq) was added at -78°C, reacted for 24h, and separated by column chromatography to obtain the target product formula L-1. Use a rotary evaporator to spin dry, add DCM to pass through celite, spin dry, add MeOH so...
Embodiment 2
[0138] Example 2 N-((2',6'-dimethoxy-[1,1'-biphenyl]-2-yl)(phenyl)phosphono)-N,P,P-triphenylene Preparation of phosphonamides
[0139]
[0140] The procedure was the same as above, and aniline was added, and ArPhPCl (3.6 g, 10.0 mmol) was added in the fourth step to obtain a white solid (3.5 g, 65%).
[0141] 1 H NMR (400MHz, CDCl 3 ):δ8.00(dd,J=11.8,7.1Hz,4H),7.34(m,8H),7.22(t,J=7.7Hz,2H),7.03(d,J=7.2Hz,2H),6.83 (t,J=7.4Hz,2H),6.78(dd,J=10.8,5.3Hz,3H),6.67(dd,J=8.0,5.2Hz,2H),3.68(s,6H). 13 C NMR (101MHz, CDCl3): δ160.7(d, J PC =18.0Hz)141.5(d,J PC =4.0Hz), 134.0(d, J PC =3.0Hz), 133.7(d,J PC =3.0Hz), 133.3(d, J PC =3.0Hz)133.2(d,J PC =3.0Hz), 131.7(d, J PC =3.0Hz), 130.9(s), 129.9(d, J PC =4.0Hz), 128.1(d, J PC =3.0Hz), 128.0(s), 125.5(s), 124.6(d, J PC =4.0Hz)124.4(d,J PC =4.0Hz), 120.6(s), 110.1(s), 55.6(s). 31 P NMR (CDCl 3 ,162MHz):δ45.7(d,J=75.3Hz),28.3(d,J=75.3Hz).ESI-MS(m / z):[M+H] + Calcd for C 32 h 30 NO 3 P 2 , 538.1701; Found: 538.1700.
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