309740-49-6

基本信息
1-甲基-4-硝基吡唑-5-甲酸甲酯
1-甲基-4-硝基-1H-吡唑-5-羧酸甲酯
1-甲基-4-硝基-1H-吡唑-5-羧酸甲酯METHYL 1-METHYL-4-NITRO-1H-PYRAZOLE-5-CARBOXYLATE
Methyl 1-Methyl-4-nitropyrazole-5-carboxylate
Methyl 1-Methyl-4-nitro-1H-pyrazole-5-carboxylate
1H-Pyrazole-5-carboxylic acid, 1-methyl-4-nitro-, methyl ester
物理化學(xué)性質(zhì)
制備方法

138786-86-4

74-88-4

400877-57-8

309740-49-6
以4-硝基-1H-吡唑-3-甲酸甲酯(2.0g,11.7mmol)和碘甲烷(2.0g,14.0mmol)為原料,在碳酸鉀(1.62g,11.7mmol)存在下,于丙酮(60mL)中,30℃下攪拌反應(yīng)5小時(shí)。反應(yīng)完成后,將混合物用水稀釋,并用氯仿進(jìn)行萃取。合并有機(jī)相,用無水硫酸鈉干燥,減壓濃縮除去溶劑。所得粗產(chǎn)物通過硅膠柱色譜法(洗脫劑:己烷-乙酸乙酯,比例從4:1至1:1)純化,分離得到兩個(gè)主要產(chǎn)物:1-甲基-4-硝基-1H-吡唑-3-羧酸甲酯(Rf值0.43,0.95g,產(chǎn)率44%)和1-甲基-4-硝基-1H-吡唑-5-羧酸甲酯(Rf值0.71,0.61g,產(chǎn)率28%)。
參考文獻(xiàn):
[1] Patent: WO2011/154327, 2011, A1. Location in patent: Page/Page column 136; 137
[2] Patent: US2010/63106, 2010, A1. Location in patent: Page/Page column 11;13
[3] Patent: WO2008/51047, 2008, A1. Location in patent: Page/Page column 25; 28-29
[4] Patent: US2009/156582, 2009, A1. Location in patent: Page/Page column 30
[5] Patent: EP1847531, 2007, A1. Location in patent: Page/Page column 43