2915-16-4

基本信息
2-氯-4,6-二苯基嘧啶
2-氯-4,6-二苯基-1,3-嘧啶
2-氯-4,6-二苯基嘧啶 2-CHLORO-4,6-DIPHENYLPYRIMIDINE
2-Chloro-4,6-diphenylpyrimidine>
Pyrimidine, 2-chloro-4,6-diphenyl-
2-chloro-4,6-diphenyl-1,3-pyrimidine
2-Chloro-4,6-diphenylpyrimidine ISO 9001:2015 REACH
物理化學性質
制備方法

3764-01-0

98-80-6

2915-16-4
以2,4,6-三氯嘧啶(PYR,1.3 mL,7 mmol)和苯硼酸(Ph-B(OH)2,1.5 g,12 mmol)為原料,在Pd(PPh3)4(0.2 g,0.17 mmol)催化下,于40 mL甲苯中混合。將混合物轉移至配備冷凝管的雙頸圓底燒瓶中,加入2 M K2CO3水溶液(40 mL)、乙醇(25 mL)和甲苯(80 mL),在氮氣保護下于110℃回流反應8小時。反應完成后,用乙酸乙酯(60 mL)和水(50 mL)萃取混合物。有機層用無水硫酸鎂干燥,過濾后濃縮。粗產物通過硅膠柱層析純化,洗脫劑為正己烷:二氯甲烷(4:1),得到中間體2P-PYR,為白色固體。進一步合成2-氯-4,6-二苯基嘧啶,產率74%;白色固體;1H NMR (500 MHz, CDCl3) δ 8.13-8.14 (m, 4H), 8.01 (s, 1H), 7.51-7.55 (m, 6H); 13C NMR (500 MHz, CDCl3) δ 167.7, 162.1, 135.7, 131.7, 129.1, 127.5, 111.0。
參考文獻:
[1] Journal of Organic Chemistry, 2001, vol. 66, # 21, p. 7125 - 7128
[2] Patent: WO2011/93609, 2011, A1. Location in patent: Page/Page column 17
[3] Patent: KR2015/92145, 2015, A. Location in patent: Paragraph 0265-0267
[4] Patent: CN103664906, 2016, B. Location in patent: Paragraph 0158; 0160
[5] Patent: CN103570628, 2016, B. Location in patent: Paragraph 0103-0106