化学合成,用于肽合成。
医药; 化学合成
合成路线 1(1. 合成:22509-74-6)
产率:79.1%
合成条件:With triethylamine In N,N-dimethyl-formamide at 20℃; for 2 h;
实验步骤:通用方法:向邻苯二甲酰亚胺(7.36g,50.00mmol)溶于无水DMF(25mL)的溶液中加入TEA(9mL,65.00mmol)。 然后将反应体系的温度冷却至0℃并滴加氯甲酸乙酯(5.7mL,60.00mmol)。 将混合物在室温下搅拌2小时并倒入冰水中,过滤。 用冷水洗涤固体并干燥,得到8.67g(79.1%收率),为白色固体。 Mp 81.4-83.6℃.1HNMR(CDCl 3,400MHz)d 1.44(s,3H,CH 3),4.48(q,J = 7.1Hz,2H,CH 2),7.80-7.85(m,2H,Ar-H), 7.93-7.99(m,2H,Ar-H)。 MS(ESI):m / z 220.1 [M + H] +。
参考文献:
- [1] Journal of Organic Chemistry, 1980, vol. 45, # 1, p. 174 - 175 [2] Organic Letters, 2015, vol. 17, # 23, p. 5846 - 5849 [3] Synthetic Communications, 1980, vol. 10, # 8, p. 611 - 614 [4] Bioorganic and Medicinal Chemistry, 2016, vol. 24, # 11, p. 2576 - 2588 [5] Patent: CN105732683, 2016, A. Location in patent: Paragraph 0090; 0091; 0092; 0093 [6] Patent: WO2013/13188, 2013, A1. Location in patent: Paragraph 00485 [7] Patent: US9416132, 2016, B2. Location in patent: Page/Page column 182; 183; 184 [8] Patent: WO2014/36022, 2014, A1. Location in patent: Paragraph 0148-0149 [9] Synthetic Communications, 1997, vol. 27, # 12, p. 2081 - 2086 [10] Journal of Medicinal Chemistry, 2013, vol. 56, # 24, p. 10003 - 10015