Photoaligning material
A technology of non-optical and optically active groups, applied in the field of photo-alignment materials, can solve problems such as undesirable, uneven surface of alignment layer, changes in electro-optical properties, etc.
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Embodiment 1
[0441] Preparation of 3,5-dinitrobenzoic acid (3β)-cholest-5-en-3-ester
[0442]
[0443] 20.00 g (51.7 mmol) of cholesterol, 2.88 g (25.75 mmol) of 4-dimethylaminopyridine, 6.27 g (62.04 mmol) of triethylamine were dissolved in 100 mL of dichloromethane. 11.92 g (51.7 mmol) of commercially available 3,5-dinitrobenzoyl chloride dissolved in 50 mL of dichloromethane were added at 0°C. The solution was stirred at 0 °C for 2 hours and at room temperature overnight. After 22 hours at room temperature, the reaction mixture was partitioned between dichloromethane and water. The organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. Crystallization from an ethyl acetate:hexane mixture afforded 16.94 g (56%) of 3,5-dinitrobenzoic acid (3β)-cholest-5-en-3-ester as yellowish crystals.
Embodiment 2
[0445] Preparation of 3,5-diaminobenzoic acid (3β)-cholest-5-en-3-ester
[0446]
[0447] 11.42 g (19.66 mmol) of 3,5-dinitrobenzoic acid (3β)-cholest-5-en-3-ester were dissolved in a mixture of 54 mL of N,N-dimethylformamide and 6 mL of water. 32.6 g (120 mmol) of ferric chloride hexahydrate were added. 13.1 g (201 mmol) of zinc powder were added in portions over 60 minutes. The mixture was allowed to react for 2 hours. The reaction mixture was partitioned between ethyl acetate and water and filtered. The organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was filtered on 400 g of silica gel using toluene:ethyl acetate 1:3 as eluent and crystallized from ethyl acetate:hexane mixture to obtain 8.20 g of 3,5-diaminobenzoic acid (3β)-cholesta-5 -en-3-ester.
[0448] 1 H NMR DMSO d 6 300MHz
[0449] 6.41(d,2H),6.01(t,1H),5.39(m,1H),4.97(s,4H),4.62(m,1H),2.36(m,2H),2.00-0.83(m,40H) ,0...
Embodiment 3
[0451] Preparation of 5-(2,4-dinitrophenyl)pentan-1-ol
[0452]
[0453] At 0°C, 50g (304mmol) 5-phenylpentan-1-ol, 127mL NEt 3 Dissolve in 50 mL THF. 46.5 g (456 mmol) of acetic anhydride were added to the mixture. The solution was stirred at 0 °C for 2 hours and at room temperature overnight. After 22 hours at room temperature, the reaction mixture was partitioned between ethyl acetate and water. The organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude product was carefully added to a mixture of 250 g sulfuric acid and 160 g nitric acid cooled at -5°C. The solution was stirred at -5°C for 2 hours. The mixture was quenched with 500 g of ice and the product was extracted with toluene. The organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The yellow oil was refluxed in 300ml methanol with 60ml HCl. After reflux f...
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