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With potassium carbonate; In N,N-dimethyl-formamide; at 20℃;
Preparation of Compound d1-2 Ethyl 7-bromoheptanoate and 3,5-bis(trifluoromethyl) phenol were added to dimethylformamide (DMF). The solution was added with potassium carbonate and stirred at room temperature. The solution was added with water and extracted twice with ethyl acetate. After the organic layer was washed three times with water and dried over anhydrous magnesium sulfate, the solvent was removed. The residue was purified by silica gel column chromatography to obtain ethyl 7-(3,5-bis (trifluoromethyl)phenoxy)heptanoate.
Step 12a: Ethyl 4-(benzyloxy)-3-(7-ethoxy-7-oxoheptyloxy)benzoate (Compound 503-20) The title compound 503-20 (1.6 g, 100%) was prepared as a yellow oil from compound 502 (4.43 g, 16.3 mmol) and ethyl 7-bromoheptanoate (1.0 g, 4.4 mmol) using a procedure similar to that described for compound 503-16 (Example 9): LCMS: 429 [M+1]+.
ethyl 7-((4-(4,6-dimorpholino-1,3,5-triazin-2-yl)phenyl)amino)heptanoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
27%
100 mg (0.29 mmol) of the compound prepared in step 1) of Example 9 was dissolved in 8 ml of N, N-dimethylformamide,After adding 23 mg (0.58 mmol) of 60% sodium hydride at 0 C and stirring at room temperature for 30 minutes, ethyl-7-bromoheptanoic acid68 [mu] l (0.35 mmol) of TEA were added. After stirring the reaction mixture at 100 & lt; 0 & gt; C for 8 hours, when the reaction is complete,Cool the mixture to room temperature. The resulting reaction mixture was added with distilled water and extracted with ethyl acetate. Separated into resultsThe organic layer was dried over anhydrous sodium sulfate and then filtered under reduced pressure and distilled under reduced pressure. The resulting residue was purified by column chromatography(Ethyl acetate: hexane = 1: 1 (volume ratio)) to obtain the title compound (40 mg, Yield 27%).
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