化学合成；材料科学。
化学合成；材料科学
合成路线 1（1. 合成：3383-83-3）
产率：100%
合成条件：With sulfuric acid; hydrogen bromide In water at 120 - 125℃; for 3 h;
实验步骤：实施例1外消旋的1-溴-3,7-二甲基辛烷（二氢吡咯烷溴化物）在搅拌下将浓硫酸（17mL）加入到48％的氢溴酸（100mL）中，然后加入3,7-二甲基辛醇（二氢硝基醇，Aldrich，67mL） 向混合物中加入100g）。 然后将混合物加热至120-125℃，并在该温度下保持3小时。 冷却反应，并萃取到庚烷（300mL）中。 用盐酸，水，碳酸氢钠溶液洗涤庚烷层，干燥并浓缩，得到81.5g油状物。 将该油状物在120-125℃的浴温下真空蒸馏，得到溴化物产物，为油状物，b.p。 85-87℃/ 10mmHg，78.2g，100％收率。 质谱：m / z 220,222（M +）。
参考文献：
- [1] Patent: US8471035, 2013, B1. Location in patent: Page/Page column 9; 10 [2] Patent: US2018/273524, 2018, A1. Location in patent: Paragraph 0044 [3] Patent: EP2816053, 2014, A1. Location in patent: Paragraph 0352 [4] Patent: US9371353, 2016, B2. Location in patent: Page/Page column 73; 74; 75 [5] Helvetica Chimica Acta, 1981, vol. 64, # 4, p. 1158 - 1173 [6] Molecular Crystals and Liquid Crystals (1969-1991), 1991, vol. 195, p. 291 - 305 [7] Patent: US2013/267697, 2013, A1. Location in patent: Page/Page column [8] Tetrahedron Letters, 2006, vol. 47, # 39, p. 7071 - 7075 [9] Archiv der Pharmazie (Weinheim, Germany), 2002, vol. 335, # 11-12, p. 535 - 546 [10] Chemical and Pharmaceutical Bulletin, 1998, vol. 46, # 9, p. 1428 - 1431 [11] Chemische Berichte, 1914, vol. 47, p. 2456 [12] Chemische Berichte, 1914, vol. 47, p. 2456 [13] Bulletin of the Chemical Society of Japan, 1975, vol. 48, p. 2317 - 2322 [14] Chemische Berichte, 1923, vol. 56, p. 2272 [15] Journal of Organic Chemistry, 1939, vol. 4, p. 340 [16] Bulletin de la Societe Chimique de France, 1937, vol. <5>4, p. 750 [17] Yakugaku Zasshi, 1952, vol. 72, p. 731,734 [18] Chem.Abstr., 1954, p. 2637 [19] Collection of Czechoslovak Chemical Communications, 1951, vol. 16/17, p. 278,281 [20] Bulletin de la Societe Chimique de France, 1929, vol. <4> 45, p. 165 [21] Tetrahedron, 1957, vol. 1, p. 186,192 [22] Journal of Natural Products, 2003, vol. 66, # 1, p. 34 - 38 [23] Patent: US5376634, 1994, A [24] Journal of Physical Chemistry A, 2011, vol. 115, # 22, p. 5525 - 5539 [25] Reactive and Functional Polymers, 2015, vol. 86, p. 67 - 79 [26] Nature Chemistry, 2016, vol. 8, # 1, p. 80 - 89 [27] Patent: US2017/342091, 2017, A1. Location in patent: Paragraph 0339; 0350
