These common heterocyclic compound, 876-53-9, name is 1,3-Dibromoadamantane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. COA of Formula: C10H14Br2
A compound of 1,3-dibromo-adamantane (3 g, 10 mmol) was dissolved in 30 mL of toluene, and then 250 mgof AIBN (1.5 mmol), 7 g of tri-n-butyl tin (24 mmol), 3 g of 2-ethyl methacrylate were added in order. The reaction wasrefluxed at 110C under nitrogen for 3 hours. The reaction solution was cooled to room temperature, and was poured into 30 mL of 0.2 M aqueous ammonia. After being stirred fully, the organic layer was separated, the aqueous layer wasextracted with ethyl acetate (20 mL34). The organic layers were combined, and washed with 30 mL of water and 30mL of saturated sodium chloride solution, dried with anhydrous sodium sulfate. The solvent was evaporated underreduced pressure to give a crude product as a colorless oil, which was separated by silica column chromatography(petroleum ether : ethyl acetate = 10:1) to obtain NM-012a as a colorless oil (1.6 g, 43.1%). ESI-MS: m/z 337.4 ([M+H]+). 1H-NMR (DMSO-d6, ppm): 0.97 (s, 2 H), 1.02-1.08 (m, 8 H), 1.15-1.20 (m, 7 H), 1.22-1.40 (m, 7 H), 1.50 (s, 2 H),1.57-1.65 (m, 2 H), 1.93 (s, 2 H), 2.39-2.47 (m, 2 H), 3.98-4.11 (m, 4 H).
The synthetic route of 1,3-Dibromoadamantane has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Guangzhou Magpie Pharmaceuticals Co., Ltd.; WANG, Yuqiang; LIU, Zheng; YU, Pei; SUN, Yewei; ZHANG, Zaijun; ZHANG, Gaoxiao; SHAN, Luchen; YI, Peng; LARRICK, James; (27 pag.)EP3150574; (2017); A1;,
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