877-42-9 6-溴-2-甲基喹啉
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分子式C10H8BrNPSA12.89 Ų外观白色至淡黄色结晶性固体或晶体粉末,常温下为固体 沸点299.7±20.0 °C (760 mmHg) 溶解度0.028 mg/ml ; 0.000126 mol/l 条件:氧气、铁(II)氯化物,对二甲苯-二甲基亚砜混合溶剂,110℃,30小时(Schlenk技术)收率:70%(8-甲基喹啉)参考文献:[1] Angewandte Chemie - International Edition, 2017, vol. 56, #11, p. 3080-3084;[2] Angew. Chem., 2017, vol. 129, #11, p. 3126-3130,5;[3] Angewandte Chemie - International Edition, 2016, vol. 55, #40, p. 12224-12227;[4] Angew. Chem., 2016, vol. 128, #40, p. 12412-12415,4;[5] Synlett, 2016, vol. 27, #12, p. 1806-1809;[6] Tetrahedron Letters, 2018, vol. 59, #10, p. 949-953;[7] Patent: CN107141252, 2017, A. Location in patent: Paragraph 0048; 0049; 0050; 0051; 0053;[8] ChemCatChem, 2017, vol. 9, #13, p. 2463-2466
- 原料:4-溴苯胺(14.59g,84.8mmol)、HCl(6N,60mL)、巴豆醛(11.9g,170mmol)
- 步骤:将4-溴苯胺与HCl混合物加热至100℃,缓慢加入巴豆醛,回流至TLC无原料;冷却后加水,EtOAc萃取未反应巴豆醛;水相中和后EtOAc萃取;有机相干燥蒸发,粗产物重结晶(EtOAc/PE)
- 条件:100℃,回流
- 收率:75.6%
- 参考文献:[1] Tetrahedron Letters, 2006, vol. 47, #11, p. 1783-1785;[2] Dyes and Pigments, 2014, vol. 101, p. 30-37;[3] Patent: WO2006/132739, 2006, A2. Location in patent: Page/Page column 37;[4] Patent: EP3239143, 2017, A2. Location in patent: Paragraph 0062;[5] Patent: WO2015/116492, 2015, A1. Location in patent: Page/Page column 78