1150271-23-0

基本信息
4-溴-1-羰基-1H-吡唑
1-BOC-4-溴-1H-吡唑
4-溴-1H-吡唑-1-甲酸叔丁酯
1-BOC-4-溴-1H-吡唑(CAS號(hào):1150271-23-0)
N-Boc-4-broMopyrazole
tert-butyl 4-bromopyrazole-1-carboxylate
t-Butyl 4-bromo-1H-pyrazole-1-carboxylate
1H-Pyrazole-1-carboxylic acid, 4-bromo-, 1,1-dimethylethyl ester
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
常見(jiàn)問(wèn)題列表

2075-45-8

24424-99-5

1150271-23-0
步驟1:制備4-溴-1H-吡唑-1-羧酸叔丁酯 在0℃下,將二碳酸二叔丁酯(Boc2O,2.34 mL,10.2 mmol)緩慢加入至4-溴-1H-吡唑(1 g,6.8 mmol)的乙腈(20 mL)溶液中。隨后,向反應(yīng)混合物中依次加入三乙胺(3.3 mL,23.8 mmol)和4-二甲基氨基吡啶(DMAP,0.166 g,1.36 mmol)。將反應(yīng)混合物在室溫下攪拌2小時(shí)。反應(yīng)完成后,用水稀釋反應(yīng)混合物,并用乙酸乙酯(100 mL × 3)進(jìn)行萃取。合并有機(jī)相,依次用水(100 mL)和飽和食鹽水(100 mL)洗滌,無(wú)水硫酸鈉干燥,減壓濃縮除去溶劑。粗產(chǎn)物通過(guò)快速柱層析(洗脫劑:10%乙酸乙酯/己烷)純化,得到4-溴-1H-吡唑-1-羧酸叔丁酯(1.65 g,收率98%)為無(wú)色液體。 1H NMR (400 MHz, CDCl3) δ 8.09 (s, 1H), 7.66 (s, 1H), 1.65 (s, 9H)。
參考文獻(xiàn):
[1] Patent: WO2016/49165, 2016, A1. Location in patent: Paragraph 00161
[2] Patent: WO2018/172250, 2018, A1. Location in patent: Page/Page column 300
[3] Patent: CN106188116, 2016, A. Location in patent: Paragraph 0016
[4] Patent: WO2014/141187, 2014, A1. Location in patent: Page/Page column 142
[5] Arkivoc, 2014, vol. 2014, # 6, p. 54 - 71