2,9-二氯-1,10-菲咯啉用于有机砌块、通用试剂。
化学合成
路线1:
- 步骤:将化合物3与五氯化磷(2当量)在氯化磷溶剂中,于110℃下反应18小时,得到目标产物;
- 条件:110℃,18小时;
- 收率:88%;
- 参考文献:[1] Beilstein Journal of Organic Chemistry, 2014, vol. 10, p. 814 - 824;[2] European Journal of Inorganic Chemistry, 2017, vol. 2017, # 34, p. 4020 - 4027;[3] Chemistry - A European Journal, 2007, vol. 13, # 27, p. 7584 - 7594;[4] Organometallics, 2013, vol. 32, # 21, p. 6511 - 6521;[5] Chemistry - A European Journal, 2014, vol. 20, # 25, p. 7819 - 7829
路线2:
- 步骤:在氩气流下,向化合物(5)(4.26g; 17.4mmol)中加入三氯氧化磷(39mL)和五氯化磷(4.48g; 21.8mmol),冰浴冷却后回流7小时,减压蒸发三氯氧化磷;向残余物中加入冰水和浓氨水至碱性,过滤、水洗、减压干燥得产物;
- 条件:氩气氛围,冰浴冷却,回流7小时,冰水/浓氨水(碱性条件);
- 收率:94%;
- 参考文献:[1] Patent: WO2011/30566, 2011, A1;[2] Patent: WO2012/124310, 2012, A1;[3] Tetrahedron Letters, 1989, vol. 30, # 4, p. 463 - 466;[4] Journal of the Indian Chemical Society, 1993, vol. 70, # 11-12, p. 877 - 884;[5] Journal of Organic Chemistry, 2000, vol. 65, # 23, p. 7757 - 7763;[6] Organic Preparations and Procedures International, 2007, vol. 39, # 6, p. 603 - 608