1224944-77-7

基本信息
5-氯吡唑并[1,5-A]嘧啶-3-羧酸乙酯 5G
thyl 5-chloropyrazolo[1,5-a]pyrimidine-3-carboxylate
Ethyl 5-chloropyrazolo[1,5-a]pyrimidine-3-carboxylate
5-Chloropyrazolo[1,5-a]pyrimidine-3-carboxylic acid ethyl este
5-Chloro-pyrazolo[1,5-a]pyrimidine-3-carboxylic acid ethyl ester
Pyrazolo[1,5-a]pyrimidine-3-carboxylic acid, 5-chloro-, ethyl ester
物理化學(xué)性質(zhì)
制備方法
![5-氧代-4,5-二氫吡唑并[1,5-a]嘧啶-3-羧酸乙酯](/CAS/GIF/926663-00-5.gif)
926663-00-5
![5-氯吡唑并[1,5-a]嘧啶-3-羧酸乙酯](/CAS/GIF/1224944-77-7.gif)
1224944-77-7
步驟B:5-氯吡唑并[1,5-a]嘧啶-3-羧酸乙酯的制備;將5-氧代-4,5-二氫吡唑[1,5-a]嘧啶-3-甲酸乙酯(22.7 g,110 mmol)懸浮于三氯氧磷(100 mL)中,加熱至回流狀態(tài)。維持回流反應(yīng)2小時(shí)后,冷卻反應(yīng)混合物,并通過(guò)減壓蒸餾除去過(guò)量的三氯氧磷。將殘余物用二氯甲烷(100 mL)稀釋?zhuān)徛谷牒斜臒恐?。分離有機(jī)層和水層,水層用二氯甲烷進(jìn)一步萃取。合并所有有機(jī)相,用無(wú)水硫酸鎂干燥,過(guò)濾后濃縮,得到5-氯吡唑并[1,5-a]嘧啶-3-羧酸乙酯(24.2 g,產(chǎn)率97.6%),為淺黃色固體。質(zhì)譜(APCI)m/z = 225.9(M + H)。
參考文獻(xiàn):
[1] Patent: WO2011/6074, 2011, A1. Location in patent: Page/Page column 70-71
[2] Chemical and Pharmaceutical Bulletin, 2017, vol. 65, # 11, p. 1058 - 1077
[3] Patent: WO2012/34095, 2012, A1. Location in patent: Page/Page column 68
[4] Patent: US2016/159808, 2016, A1. Location in patent: Paragraph 1357; 1358; 1381; 1382; 1394; 1395
[5] Patent: TW2016/520, 2016, A. Location in patent: Paragraph 0165