114435-86-8

基本信息
4-甲基苯磺酸氟甲酯
4-氟甲基苯磺酸甲酯
氟甲基-4-甲基苯磺酸酯
4-甲基苯磺酸(氟甲基)酯
luoroMethyl 4-Methylbenzenesulfonate
fluoroMethyl 4-Methylbenzenesulfonate
Fluoromethyl 4-methylbenzenesulfonate 97+%
Methanol, fluoro-, 4-methylbenzenesulfonate
Methanol, 1-fluoro-, 1-(4-methylbenzenesulfonate)
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法
![1-甲基-4-[(4-甲基苯基)磺酰氧基甲氧基磺酰基]苯](/CAS/GIF/24124-59-2.gif)
24124-59-2

114435-86-8
以亞甲基雙(4-甲基苯磺酸酯)為原料合成氟甲基-4-甲基苯磺酸酯的一般步驟:將亞甲基雙(4-甲基苯磺酸酯)(100 mg,0.28 mmol)和氟化銫(213 mg,1.4 mmol)溶解于叔戊醇(5 mL)中,置于微波反應(yīng)器中,于90℃下反應(yīng)15分鐘。反應(yīng)完成后,冷卻至室溫,減壓蒸餾除去叔戊醇。向殘余物中加入冰冷的乙醚,過濾所得懸浮液,并用大量冰冷的乙醚洗滌固體。濾液經(jīng)減壓濃縮,得到4-甲基苯磺酸氟甲酯,為無色油狀物(49 mg,收率88%)。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR(500 MHz,CDCl3)δ:2.43(s,3H,ArCH3),5.72(d,2H,CH2,J = 51.0 Hz),7.35(d,2H,ArH,J = 8.0 Hz),7.81(d,2H,ArH,J = 8.0 Hz);13C NMR(125 MHz,CDCl3)δ:21.67,98.16(d,J = 221 Hz),127.87,129.96,133.77,145.63;19F NMR(471 MHz,CDCl3)δ:-153.24(t,J = 50.7 Hz)確認(rèn)。
參考文獻(xiàn):
[1] Tetrahedron Letters, 2018, vol. 59, # 17, p. 1635 - 1637
[2] Bioorganic and Medicinal Chemistry Letters, 2015, vol. 25, # 18, p. 3956 - 3960
[3] Journal of Labelled Compounds and Radiopharmaceuticals, 2003, vol. 46, # 6, p. 555 - 566
[4] ChemMedChem, 2016, vol. 11, # 1, p. 108 - 118
[5] Patent: WO2012/40133, 2012, A2. Location in patent: Page/Page column 36-37