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With pyridine; titanium(IV) isopropylate In tetrahydrofuran at 60℃; for 5h; Inert atmosphere;
5
2-nonanone (2.66 g, 20 mmol) and 4,4'-dimethoxybenzophenone (5.81 g, 24 mmol) were dissolved.In 100 mL of THF, followed by the addition of pyridine (3.2 mL, 40 mmol), tetraisopropyl titanate (IV) (17.8 mL, 60 mmol), mixtureThe reaction was carried out at 60 ° C for 5 h under N2 protection, and the THF was spun dry using a vacuum rotary evaporator, then dissolved in DCM/H2O and extracted with a Buchner funnel.The filtrate was extracted three times, and the DCM layer was concentrated, and then purified by column chromatography to obtain a gold-yellow solid INDO-DOMe (aggregation-inducing luminescent material) with a yield of 5.53 g and a yield of 77.3%.
55%
With sodium hydride In tetrahydrofuran for 120h; Heating / reflux;
65
NaH (50% dispersion in oil, 50 mg, 1 mmole) was added in one portion to a solution of 1, 3-dihydro-indol-2-one (130 mg, 1 mmole) in dry THF (5 mL). When the resulting gas evolution ceased bis- (4-methoxy-phenyl)-methanone (290 mg, 1.2 mmoles) was added in one portion. The reaction mixture was heated to reflux for about 3 days. Extra portions of NaH (in total 75 mg, 1.5 mmoles) were added over the next 2 days. H20 was then added (10 mL) and the pH of the crude was adjusted to 6-7 by addition of cold acetic acid. Crystals formed which were filtered and recrystallized from MeOH to afford 200 mg of the pure title compound (55% yield) (DMSO-d6) til037 (slH) 718 (m4H) 704 (m3H) 688 (d2H) 675 (d, lH), 6. 59 (t, lH), 6. 27 (d, lH), 3. 83 (s, 3H), 3. 79 (s, 3H).
55%
With pyridine; titanium(IV) isopropylate In tetrahydrofuran at 60℃; for 10h;
With [1,3-dibenzylbenzimidazol-2-ylidene]dichlorido(η6-p-cymene)ruthenium(II); caesium carbonate In 1,4-dioxane at 140℃; for 48h; Inert atmosphere; Sealed tube;