2-溴-1-(4-溴-2-氟苯基)乙酮是一种重要的有机合成中间体,广泛应用于医药和农药等领域的精细化工合成过程中。
医药; 农药
合成路线 1(869569-77-7)
- 步骤: 将2-溴-1-(4-溴-2-氟苯基)乙酮溴(1.2 mL,23.0 mmol)在10 mL冰醋酸中的溶液滴加到1-(4-溴-2-氟苯基)乙酮(5.0 g,23.0 mmol)在150 mL无水二氯甲烷中的溶液中,0℃下反应;滴加完毕后,使反应混合物温热至室温。
- 条件: 反应在0 - 20℃下进行,使用溴(Br₂)和冰醋酸(AcOH)作为试剂,无水二氯甲烷(CH₂Cl₂)作为溶剂。
- 监测: 通过TLC(5%乙酸乙酯:己烷)监测反应进程,确认原料消耗完全。
- 后处理: 反应混合物用二氯甲烷稀释,依次用5%硫代硫酸钠溶液和盐水洗涤;有机层经无水硫酸钠干燥、过滤后减压浓缩。
- 产率: 得到2-溴-1-(4-溴-2-氟苯基)乙酮(6.6 g,收率97%),产物为浅绿色油状物。
- 参考文献: [1] Patent: US2008/45556, 2008, A1. Location in patent: Page/Page column 32-33;[2] Patent: WO2012/125926, 2012, A2. Location in patent: Page/Page column 79;[3] Patent: WO2012/122716, 2012, A1. Location in patent: Page/Page column 98;[4] Patent: CN107629023, 2018, A. Location in patent: Paragraph 0199; 0202; 0203; 0204;[5] Patent: CN107629022, 2018, A. Location in patent: Paragraph 0311; 0312; 0313; 0314;[6] Patent: WO2005/107762, 2005, A2. Location in patent: Page/Page column 260-262;[7] Patent: WO2007/56056, 2007, A2. Location in patent: Page/Page column 68;[8] Patent: WO2009/151991, 2009, A1. Location in patent: Page/Page column 149;[9] Patent: WO2012/109080, 2012, A1. Location in patent: Page/Page column 53-54;[10] Patent: WO2012/154777, 2012, A1. Location in patent: Page/Page column 110;[11] Patent: WO2013/162077, 2013, A1. Location in patent: Paragraph 0483;[12] Patent: WO2014/65791, 2014, A1. Location in patent: Page/Page column 127;[13] Patent: US2008/44380, 2008, A1. Location in patent: Page/Page column 164