889877-77-4
889877-77-4 結(jié)構(gòu)式
基本信息
(7R)-2-氯-7-乙基-7,8-二氫-8-(1-甲基乙基)-6(5H)-蝶啶酮
Volasertib(BI6727)-A4
Thiazole,2-bromo-8-(bromomethyl)-
2-Chloro-7-ethyl-8-isopropyl-7,8-dihydro-5H-pteridin-6-one
(R)-2-Chloro-7-ethyl-8-isopropyl-7,8-dihydro-5H-pteridin-6-one
(R)-2-chloro-7-ethyl-8-isopropyl-7,8-dihydropteridin-6(5H)-one
(7R)-2-Chloro-7-ethyl-7,8-dihydro-8-(1-methylethyl)-6(5H)-pteridinone
6(5H)-Pteridinone, 2-chloro-7-ethyl-7,8-dihydro-8-(1-methylethyl)-, (7R)-
制備方法
946161-16-6
889877-77-4
以 (R)-2-((2-氯-5-硝基嘧啶-4-基)(異丙基)氨基)丁酸甲酯為原料合成 (R)-2-氯-7-乙基-8-異丙基-7,8-二氫蝶啶-6(5H)-酮的一般步驟：將50g (R)-2-((2-氯-5-硝基嘧啶-4-基)(異丙基)氨基)丁酸甲酯溶解于375mL四氫呋喃中，在5g 鉑碳催化劑（5％負(fù)載量）存在下，于3巴氫氣壓力和35℃條件下進(jìn)行氫化反應(yīng)，直至氫氣消耗停止。隨后加入2.5g乙酰丙酮氧釩，繼續(xù)氫化反應(yīng)。反應(yīng)完成后，過濾反應(yīng)混合物以移除催化劑。通過減壓蒸餾除去溶劑。向殘留物中加入150mL 2-丙醇，加熱至回流狀態(tài)。然后加入300mL去離子水，將所得懸浮液緩慢冷卻至2℃。通過抽濾收集沉淀，并用冷的2-丙醇與去離子水混合液洗滌。最后，將產(chǎn)物在50℃真空干燥箱中干燥，得到36g (R)-2-氯-7-乙基-8-異丙基-7,8-二氫蝶啶-6(5H)-酮，收率為理論值的90%。
參考文獻(xiàn)：
[1] Patent: WO2007/90844, 2007, A1. Location in patent: Page/Page column 13
[2] Patent: WO2009/19205, 2009, A1. Location in patent: Page/Page column 13-14
[3] Bioorganic and Medicinal Chemistry Letters, 2017, vol. 27, # 5, p. 1311 - 1315
[4] Patent: EP2481739, 2012, A1. Location in patent: Page/Page column 57
[5] Patent: US2012/184543, 2012, A1. Location in patent: Page/Page column 59