13330-65-9 2,4-二甲氧基苯酚

运输信息：常温运输。危险描述：非危险化学品，海关编码2909500090

化学合成

化学合成

合成路线 1（1. 合成：13330-65-9）

• 步骤：向0.5mL甲酸中滴加2,4-二甲氧基苯甲醛（5.0g / 30mmol）和5mL 30％H₂O₂在50mL甲醇中的溶液，室温搅拌20小时；蒸发约45mL甲醇，二氯甲烷与蒸馏水分配，水相用3×50mL二氯甲烷萃取，有机相用3×50mL蒸馏水洗涤，无水硫酸钠干燥，过滤蒸发有机溶剂，柱色谱（氯仿）纯化。
• 条件：With sulfuric acid; dihydrogen peroxide In methanol at 20℃; for 20 h;
• 产率：94%
• 参考文献：[1] European Journal of Medicinal Chemistry, 2013, vol. 69, p. 798 - 816 [2] Journal of Organic Chemistry, 1984, vol. 49, #24, p. 4740 - 4741 [3] Organic Letters, 2012, vol. 14, #11, p. 2806 - 2809 [4] Tetrahedron Letters, 1999, vol. 40, #15, p. 3037 - 3040 [5] Journal of the Chemical Society, Perkin Transactions 1, 2000, #5, p. 799 - 811 [6] Organic Letters, 2011, vol. 13, #12, p. 3126 - 3129 [7] Journal of the American Chemical Society, 2012, vol. 134, #7, p. 3571 - 3576 [8] Chemistry Letters, 1995, #2, p. 127 - 128 [9] Organic and Biomolecular Chemistry, 2009, vol. 7, #24, p. 5059 - 5062 [10] Indian Journal of Chemistry, Section B: Organic Chemistry Including Medicinal Chemistry, 1994, vol. 33, #11, p. 1103 - 1104 [11] Chemistry - A European Journal, 2004, vol. 10, #17, p. 4115 - 4125 [12] Organic Letters, 2003, vol. 5, #21, p. 3859 - 3862 [13] Journal of Organic Chemistry, 2011, vol. 76, #21, p. 9151 - 9156 [14] Chemische Berichte, 1940, vol. 73, p. 795,802 [15] Chemische Berichte, 1940, vol. 73, p. 935,937 [16] Tetrahedron, 1968, vol. 24, p. 2617 - 2622 [17] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1993, #10, p. 1153 - 1160 [18] Synthesis, 1989, #3, p. 167 - 172 [19] Journal of the American Chemical Society, 1950, vol. 72, p. 4986 [20] Heterocycles, 2013, vol. 87, #8, p. 1727 - 1739