Up-regulator for expression of ATP (adenosine triphosphate)-binding cassette transporter A1 and application thereof
A technology of transporters and uses, applied in the field of medicine, can solve problems such as ineffectiveness
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preparation example 1
[0072] Preparation Example 1: Preparation of Compound Ia
[0073]
[0074] Take 1.22g (0.01mol) of p-hydroxybenzaldehyde, 15mL of dioxane, 5mL of water, and 0.44g (0.011mol) of sodium hydroxide in a 50mL round bottom flask. The reaction is exothermic. After stirring for 0.5h, let it cool to At room temperature, add chloroethanol (3 mL, excess), reflux for 3 h, cool to room temperature, extract with ether, wash twice with water, dry with anhydrous sodium sulfate, evaporate the solvent under reduced pressure, and obtain a light yellow solid Ia by column chromatography , Yield 1.35g, yield 81%. IR(KBr,cm -1 )ν: 3370, 1684, 1600, 1509, 1309, 1164, 1112, 1034, 839; 1 H NMR (CDCl 3 ,300MHz)δ:9.89(s,1H,CHO),7.79(d,J=8.3Hz,2H,ArH),7.32(d,J=8.4Hz,2H,ArH),4.75(t,2H,CH 2 ),4.42(t,2H,CH 2 ).
preparation example 2
[0075] Preparation Example 2: Preparation of Compound Ib
[0076]
[0077] Step (1): Take 6g (0.05mol) of ethylene glycol monobutyl ether, 4g of sodium hydroxide, and 10mL of water in a 50mL round-bottomed flask, stir in an ice bath for half an hour, control the temperature at 0°C, and use a constant pressure dropping funnel to Slowly add 20 mL of a THF solution in which 20.96 g (0.11 mol) of TsCl was dissolved. Continue to react for 5h. Then add 2M NaOH 20mL and heat up to 60°C to react for half an hour to remove excess TsCl, extract with chloroform, dry over anhydrous magnesium sulfate, and evaporate to dryness to obtain a colorless transparent viscous liquid, namely ethylene glycol monobutyl ether sulfonate, yield 11.88g, yield The rate is 92%. 1 H NMR (CDCl 3 ,300MHz)δ:7.79(d,J=8.3Hz,2H,ArH),7.32(d,J=8.4Hz,2H,ArH),4.60(t,2H,CH 2 ),4.15(t,2H,CH 2 ),3.40(t,2H,CH 2 ),2.44(s,3H,CH 3 ),1.50-1.43(m,2H,CH 2 ),1.34-1.26(m,2H,CH 2 ),0.89(t,3H,CH 3 ).
[0078] Step (...
preparation example 3
[0079] Preparation Example 3: Preparation of Compound Ic
[0080]
[0081] The title compound was prepared with reference to the method of Preparation Example 2, using diethylene glycol monomethyl ether instead of ethylene glycol monobutyl ether, and condensed with p-hydroxybenzaldehyde to obtain 4-(2-(2-methoxyl) shown in formula Ic Ethoxy)ethoxy)benzaldehyde: pale yellow low-melting solid, yield 1.62g, yield 73%, mp.44-45°C. IR(KBr,cm -1 )ν: 2891, 1689, 1601, 1509, 1129, 1104, 1034, 836; 1 H NMR (CDCl 3 ,300MHz)δ:9.89(s,1H,CHO),7.81(d,J=8.7Hz,2H,ArH),7.02(d,J=8.6Hz,2H,ArH),4.23(t,J=5.0Hz ,2H,CH 2 ),3.90(t,J=4.7Hz,2H,CH 2 ),3.73(dd,J=2.0Hz,4.8Hz,2H,CH 2 ),3.59(dd,2H,J=2.0Hz,4.8Hz,CH 2 ),3.34(s,3H,CH 3 );ESI-MS: m / z223(M+1,82).
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