文献类型：专利

英文题名：Preparation of 2-(1-adamantyl)-4-bromophenol involves soaking sodium-type positive ion exchange resin or H-type strong acid ion exchange resin catalyst, washing resin with deionized water, distilling mother liquor and cooling

作者：WANG N;WANG R;ZOU G

机构：[1]UNIV EAST CHINA SCI&TECHNOLOGY

申请号：CN101955417-B

公开日：2013-01-02

语种：英文

收录：DERWENT

摘要：NOVELTY - A sodium-type positive ion exchange resin is soaked, filtered and resin is washed with deionized water. H-type strong acid positive ion exchange resin is soaked, extracted, filtered and dried to obtain H-type strong acid ion exchange resin catalyst. 1-Adamantanol, para-bromophenol and glacial acetic acid are added and stirred to obtain product. The obtained product is reacted, acetic anhydride is added into reaction mixture, mother liquor is distilled, acetic acid is recycled, residual solid is re-crystallized and cooled to obtain 2-(1-adamantyl)-4-bromophenol. USE - Preparation of 2-(1-adamantyl)-4-bromophenol. ADVANTAGE - The method is environmentally-friendly and provides 2-(1-adamantyl)-4-bromophenol with high yield (92-99%) and purity (99%), by a simple process. DETAILED DESCRIPTION - A sodium-type positive ion exchange resin is soaked for 12 hours having sulfuric acid aqueous solution (30%), filtered and resin is washed with deionized water until rinsed water is neutral. A H-type strong acid positive ion exchange resin is soaked with acetic acid for 1 hour, extracted and filtered, repeatedly soaked, extracted and filtered, vacuum is carried out and dried at 100 degrees C for 3 hours to obtain H-type strong acid ion exchange resin catalyst. 1-Adamantanol (in parts weight) (1), para-bromophenol (1.1), H-type strong acid ion exchange resin catalyst (2) and glacial acetic acid (5) are added into a reactor which is provided with mechanical stirring device, heated at 100 degrees C and stirred to obtain product. The obtained product is reacted for 3-5 hours, cooled to room temperature, acetic anhydride (0.65) is added into reaction mixture and filtered for recycling ion exchange resin to obtain product. The mother liquor is distilled and acetic acid is recycled, residual solid is thermally re-crystallized with petroleum ether (6) at 60-90 degrees C and cooled to room temperature for separating to obtain 2-(1-adamantyl)-4-bromophenol.