A kind of indoline compound and its application
A compound, indoline technology, applied in the field of dye compounds, can solve problems such as limited application, narrow light capture range, and poor planarity of compounds
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Embodiment 1
[0025] Embodiment 1 is synthesized (R 1 =R 2 =CH 3 )
[0026]
[0027] Add 5.00g (23.26mmol) of compound 1 and 6.64g (28.99mmol) of compound 2 into a 250mL single-necked flask, add 150mL of methanol, install a water trap and stir at reflux at 70° for 24 hours to stop the reaction. After the solvent was spin-dried, the reactant was washed with water several times, extracted with ethyl acetate, and the ethyl acetate layer was spin-dried and purified by column chromatography to obtain 5.5 g of oily compound 2. 1 HNMR (500Hz, CDCl 3 ): 7.61(s,1H),7.54(d,J=8.0Hz,1H),7.15(d,J=8.0Hz,1H),3.94(s,3H),2.35(s,3H).
[0028]
[0029] Add 2.29g (1.00mmol) compound 2 and 1.57g (1.00mmol) compound 3, Cu powder 0.64g (1.00mmol), 1.9gCuI (1.00mmol), K 2 CO 3 Solid 2.07g (1.5mmol), 50mL o-dichlorobenzene, heated to 180° under nitrogen protection, refluxed and stirred for 24-48 hours. After the reaction was completed, the solvent was distilled off under reduced pressure. use CH 2 Cl...
Embodiment 2
[0036] Embodiment 2 is synthesized (R 1 =CH 3 , R 2 =C 8 h 17 )
[0037]
[0038] Add 1.00 g of compound 5 into a single-necked round bottom flask, take 10 mL of n-octylmagnesium bromide, stir and reflux for 12 h under deoxygenation and nitrogen protection, wash the reaction solution with saturated ammonium chloride solution and extract with ethyl acetate, spin dry and pass through the column Purification yielded 0.60 g of compound 8. 1 H NMR (500Hz, CDCl 3 ): 7.89(s, 1H), 7.18(d, J=7.5Hz, 1H), 7.12(d, J=8.5Hz, 1H), 6.99-7.02(m, 2H), 6.88(t, J=7.5Hz ,1H),6.24(d,J=8.5Hz,1H),4.53(t,J=8.5Hz,1H),3.98(t,J=8.5Hz,1H),2.40(s,3H),2.06-2.08 (m,1H),1.80-1.85(m,5H),1.46-1.52(m,10H),1.31-1.38(m,18H),0.90(t,J=8.5Hz,6H).
[0039]
[0040] Add 0.11g of compound 8 to a 25mL single-necked bottle, add 0.4g of cation exchange resin Amberlyst 15, add 15mL of toluene and install a water separator device, stir and reflux for 12h, the reactant is suction filtered, the filtrate is spin-d...
Embodiment 3
[0041] Embodiment 3 applies compound 7 to synthetic sensitizing dyes
[0042]
[0043] Add 0.51g of compound 7 to a 100mL single-necked bottle, and use CH 2 Cl 2 Dissolve, add 0.41g N-bromosuccinimide solution dissolved in acetonitrile to a constant pressure dropping funnel under ice bath, react in the dark for 3 hours, wash the reaction solution with water, extract with ethyl acetate, spin dry, and purify by column to obtain 0.43g of compound 10 , yield 66.48%. 1 H NMR (500Hz, Acetone-d6): 7.25-7.28 (m, 2H), 7.12 (s, 1H), 6.99 (d, J=8.0Hz, 1H), 6.70 (d, J=8.0Hz, 1H), 4.70(t, J=8.5Hz, 1H), 3.98(t, J=8.5Hz, 1H), 2.29(s, 3H), 2.05-2.14(m, 2H), 1.98-2.01(m, 2H), 1.82 -1.87(m,2H),1.70(s,3H),1.43(s,3H).
[0044]
[0045] Dissolve 0.2g (0.54mmol) of compound 10 in dry THF into a 50mL three-neck flask, stir the reaction substrate under nitrogen protection until the temperature drops to -78°, slowly add 2mL of n-BuLi dropwise and stir for 1-2h, Slowly add 0.51g (2.71mmol) t...
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