87808-48-8

基本信息
Methyl 3-fluoro-4-methybenzoate
METHYL 3-FLUORO-4-METHYLBENZOATE
3-Fluoro-4-methyl-Benzoic acid methyl ester
Benzoic acid, 3-fluoro-4-methyl-, methyl ester
物理化學(xué)性質(zhì)
制備方法

67-56-1

350-28-7

87808-48-8
步驟1:3-氟-4-甲基苯甲酸甲酯的合成:將3-氟-4-甲基苯甲酸(20g,130mmol)溶解于亞硫酰氯(80ml)中,加熱回流2小時(shí)(通過TLC監(jiān)測反應(yīng)至原料完全消失)。隨后,減壓蒸餾除去過量的亞硫酰氯。將殘余物冷卻至0℃,在攪拌下緩慢滴加甲醇(100ml)。滴加完畢后,將反應(yīng)混合物于室溫下繼續(xù)攪拌1小時(shí)。反應(yīng)完成后,減壓濃縮反應(yīng)混合物,用乙酸乙酯稀釋,并用飽和食鹽水洗滌。有機(jī)層經(jīng)無水硫酸鈉干燥,過濾后減壓濃縮,得到3-氟-4-甲基苯甲酸甲酯,為白色固體,無需進(jìn)一步純化即可直接用于后續(xù)反應(yīng)(產(chǎn)量:21g,收率:96%)。
參考文獻(xiàn):
[1] Organic Process Research and Development, 2008, vol. 12, # 6, p. 1137 - 1141
[2] Patent: WO2011/100433, 2011, A1. Location in patent: Page/Page column 56
[3] Patent: WO2014/102376, 2014, A1. Location in patent: Page/Page column 44-45
[4] Patent: WO2014/102377, 2014, A1. Location in patent: Page/Page column 49
[5] Patent: WO2012/80221, 2012, A1. Location in patent: Page/Page column 82