53606-06-7 4-(甲磺酰基)苄溴

运输信息：常温运输。危险描述：危险品运输编号UN3261，WGK Germany:3，危险等级8，包装类别III，海关编码29049090，存储类别11 - 可燃固体，危险性类别急性毒性类别4（经口）、眼部刺激类别2，包装等级III。

化学合成

化学合成

路线1：

• 步骤: 在0℃下向搅拌的（4-（甲基磺酰基）苯基）甲醇和三乙胺的丙酮溶液中加入甲磺酰氯，滴加后搅拌30分钟；过滤反应混合物，在0℃下向滤液中分三批加入溴化锂，搅拌5分钟后升温至室温继续搅拌1.5小时；过滤，滤液真空浓缩，用水稀释后用二氯甲烷萃取，合并有机相干燥并浓缩得到产物。
• 条件: Stage #1: With methanesulfonyl chloride; triethylamine In acetone at 0℃; for 0.50 h; Stage #2: With lithium bromide In acetone at 0 - 20℃; for 1.58 h;
• 收率: 100%
• 参考文献: [1] Patent: WO2017/136871, 2017, A1. Location in patent: Paragraph 0223 [2] Journal of the Chemical Society, 1962, p. 1420 - 1427 [3] Canadian Journal of Chemistry, 1984, vol. 62, p. 2330 - 2336 [4] Journal of Medicinal Chemistry, 1989, vol. 32, # 8, p. 1757 - 1763 [5] Journal of Organic Chemistry, 2011, vol. 76, # 20, p. 8203 - 8214

路线2：

• 步骤: 将1-甲磺酰基-4-甲基-苯、N-溴代琥珀酰亚胺和过氧化苯甲酰在四氯化碳中搅拌混合物加热回流4小时；冷却后过滤并真空浓缩，残余物经色谱分离得到产物。
• 条件: With N-Bromosuccinimide; dibenzoyl peroxide In tetrachloromethane for 4 h; Heating / reflux
• 收率: 38%
• 参考文献: [1] Synlett, 2003, # 5, p. 702 - 704 [2] Patent: WO2008/49047, 2008, A2. Location in patent: Page/Page column 121 [3] Zhurnal Obshchei Khimii, 1958, vol. 28, p. 488,494; engl. Ausg. S. 480, 484 [4] Journal of the Chemical Society, 1962, p. 1420 - 1427 [5] Journal of the Chemical Society, 1962, p. 1420 - 1427 [6] Journal of Organic Chemistry, 1975, vol. 40, # 25, p. 3778 - 3780 [7] Tetrahedron, 1984, vol. 40, # 10, p. 1863 - 1868 [8] Journal of Heterocyclic Chemistry, 1994, vol. 31, # 4, p. 1005 - 1010 [9] Organic Letters, 2013, vol. 15, # 16, p. 4194 - 4197 [10] European Journal of Organic Chemistry, 2014, vol. 2014, # 16, p. 3402 - 3410