N-(4-substituted phenylethyl)acetamide compounds and their use
A technology of amide compounds and phenethyl, applied in the field of N-acetamide compounds
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[0041] The method for the compound shown in the preparation formula I provided by the invention specifically comprises the following steps:
[0042] (1) the carboxylic acid (R 2 COOH) was dissolved in dichloromethane and added 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and 1-hydroxybenzotriazole under stirring, reacted at room temperature for 1 hour and then added N , N-diisopropylethylamine, 4-dimethylaminopyridine, add 4-nitrophenethylamine hydrochloride, then react at room temperature for 24 hours, stop the reaction, add water to the reaction solution, and use ethyl acetate Esters were extracted, concentrated, and the solvent was distilled off under reduced pressure, the residue was washed with water, and then extracted with ethyl acetate, and the organic phase was purified by silica gel column chromatography to obtain the compound shown in formula II;
[0043] (2) the compound shown in formula II is dissolved in methanol, under stirring, add 10% palladium c...
Embodiment 1
[0049] N-(4-(((2,4-diaminopyrimidin-5-yl)methyl)amino)phenethyl)-2,3-dihydrobenzo[b][1,4]dioxin- 6-formamide (marked as "I A -1") Preparation:
[0050] (1) Preparation of N-(4-nitrophenethyl)-2,3-dihydrobenzo[b][1,4]dioxin-6-carboxamide (compound shown in formula II-1) :
[0051]
[0052] Dissolve 1.80g (10mmol) of 1,4-benzodioxane-6-carboxylic acid in 50ml of dichloromethane, and add 3.8g (20mmol) of 1-ethyl-(3-dimethylaminopropyl) under stirring ) carbodiimide hydrochloride, 2.7g (20mmol) 1-hydroxybenzotriazole, after reacting at room temperature for 1h, add 3.3mL (20mmol) N,N-diisopropylethylamine, 0.122g (1mmol) 4-Dimethylaminopyridine, add 2.03g (10mmol) 4-nitrophenethylamine hydrochloride, react at room temperature for 24h, then add an appropriate amount of water, extract with ethyl acetate, wash the organic phase with saturated brine, and concentrate the organic phase. phase (removal of solvent by distillation under reduced pressure), and the residue was separate...
Embodiment 2
[0069] N-(4-(((2,4-diaminopyrimidin-5-yl)methyl)amino)phenethyl)benzo[d][1,3]dioxolane (labeled " I A -2") Preparation:
[0070] In addition to replacing 1,4-benzodioxane-6-carboxylic acid with benzo[d][1,3]dioxolanecarboxylic acid in step (1) of Example 1, all other Need raw material, reagent and preparation method with embodiment 1, obtain white solid (I A -2), yield 50%.
[0071] 1H NMR (400MHz, DMSO) δ8.35(t, J=5.5Hz, 1H), 7.64(s, 1H), 7.41(dd, J=8.1, 1.7Hz, 1H), 7.36(d, J=1.6Hz ,1H),6.95(dd,J=15.1,8.3Hz,3H),6.52(d,J=8.4Hz,2H),6.46(s,1H),6.08(s,2H),6.03(s,2H) ,5.68(s,1H),3.89(d,J=5.2Hz,2H),3.34(s,3H),2.71–2.59(m,2H).
[0072] HRMS(EI)m / z calce C 21 h 22 N 6 o 3 (M + ) 406.1753 (theoretical value), found 406.1753.
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