Synthetic method of 2-(4-tertbutyloxycarbonyl-piperazinyl)-2-(1-naphthyl)acetic acid
A technology of tert-butoxycarbonyl and synthetic method, applied in the synthesis field of 2-(4-tert-butoxycarbonyl-piperazinyl)-2-(1-naphthyl)acetic acid, can solve the problem that no effective synthetic method has been found, etc. problem, to achieve the effect of cheap reagents and simple reaction conditions
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Embodiment 1
[0009] step 1:
[0010] Add methyl 1-naphthaleneacetate (21.0 g, 105 mmol), carbon tetrachloride (200 mL), N-bromosuccinimide (20.6 g, 115.5 mmol) and benzoyl peroxide into a three-necked flask (2.5 g, 10.5 mmol). The reaction solution was stirred at 80°C for 2 hours. The reaction solution was cooled to room temperature, filtered to remove the solid, and the filtrate was spin-dried; the residue was dissolved in ethyl acetate (200 mL), and successively washed with 10% citric acid aqueous solution (50 mL) and saturated sodium bicarbonate aqueous solution (50 mL ) and saturated saline (50 mL); dried over sodium sulfate and filtered. The filtrate was spin-dried to obtain a brown liquid, compound 1 (26.0 g, 93.2 mmol, 89%). 1 H NMR (400 MHz, CDCl 3 ): 8.10 (m, 1H), 7.87 (m, 2H), 7.77 (m, 1H), 7.56(m, 1H), 7.53 (m, 1H), 7.46 (m, 1H), 6.17 (s, 1H) , (s, 3H) ppm. LC-MS (ESI): m / z 279.32 [M+H] + ;
[0011] Step 2:
[0012] Add compound 1 (26.0 g, 93.2 mmol), N,N-dimethylformami...
Embodiment 2
[0015] Example 2, step 1: methyl 1-naphthalene acetate neutralizes N-bromosuccinimide in carbon tetrachloride, the reaction time of benzoyl peroxide is 1 hour, and the reaction temperature is 90°C; the rest are implemented in the same way example 1.
Embodiment 3
[0016] Example 3, step 1: methyl 1-naphthalene acetate neutralizes N-bromosuccinimide in carbon tetrachloride, the reaction time of benzoyl peroxide is 3 hours, and the reaction temperature is 70°C; the rest are implemented in the same way example 1.
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