934524-10-4
934524-10-4 結(jié)構(gòu)式
基本信息
2,4-二氯-7-對(duì)甲苯磺酸-7H-吡咯并[2,3-D]嘧啶
2,4-二氯-7-對(duì)甲基苯磺酰基-7H-吡咯[2,3-D]嘧啶
2,4-二氯-7-對(duì)甲苯磺?;?7H-吡咯并[2,3-D]嘧啶
2,4-二氯-7-(甲苯-4-磺酰)-7H-吡咯并[2,3-D]嘧啶
2,4-Dichloro-7-tosyl-7H-pyrrolo[2,3-d]pyriMidine
2,4-Dichloro-7-(p-tolylsulfonyl)pyrrolo[2,3-d]pyrimidine
2,4-dichloro-7-(4-methylphenyl)sulfonylpyrrolo[2,3-d]pyrimidine
2,4-Dichloro-7-(toluene-4-sulfonyl)-7H-pyrrolo[2,3-d]pyriMidine
2,4-dichloro-7-(4-methylbenzenesulfonyl)-7H-pyrrolo[2,3-d]pyrimidine
2,4-Dichloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidine
7H-Pyrrolo[2,3-d]pyriMidine, 2,4-dichloro-7-[(4-Methylphenyl)sulfonyl]-
物理化學(xué)性質(zhì)
制備方法
90213-66-4
98-59-9
934524-10-4
以2,4-二氯-7H-吡咯并[2,3-d]嘧啶(1.00 g,5.32 mmol)和對(duì)甲苯磺酰氯(1.115 g,5.85 mmol)為原料,在室溫下,將兩者與硫酸氫四丁基銨(0.090 g,0.27 mmol)一同溶解于二氯甲烷(20 mL)中。隨后,向反應(yīng)混合物中加入50%氫氧化鈉水溶液(1 mL),并在室溫下攪拌30分鐘。通過薄層色譜(TLC)監(jiān)測(cè)反應(yīng)進(jìn)度,確認(rèn)反應(yīng)完成后,用去離子水和二氯甲烷稀釋反應(yīng)混合物,分離有機(jī)層。有機(jī)層經(jīng)真空蒸發(fā)濃縮,得到淺黃色固體。該粗產(chǎn)物通過柱色譜法(100%二氯甲烷作為洗脫劑)純化,得到目標(biāo)產(chǎn)物2,4-二氯-7-甲苯磺酰-7H-吡咯并[2,3-d]嘧啶(1.76 g,收率97%),為白色固體。質(zhì)譜(LCMS)顯示:[M + H]+ m/z 342。1H NMR(400 MHz,氯仿-d)δ ppm:8.14(d,J = 8.59 Hz,2H),7.78(d,J = 3.79 Hz,1H),7.39(d,J = 8.59 Hz,2H),6.70(d,J = 3.79 Hz,1H),2.45(s,3H)。
參考文獻(xiàn):
[1] Patent: WO2010/38060, 2010, A1. Location in patent: Page/Page column 68-69
[2] Journal of Medicinal Chemistry, 2014, vol. 57, # 1, p. 144 - 158
[3] Patent: WO2010/123919, 2010, A2. Location in patent: Page/Page column 55
[4] Patent: WO2017/106771, 2017, A1. Location in patent: Paragraph 00397
[5] Patent: WO2017/133667, 2017, A1. Location in patent: Page/Page column 400