33301-41-6

基本信息
1-二苯甲基氮雜環(huán)丁-3-基甲磺酸酯
1-BENZHYDRYL-3-METHANESULFONYLOXY AZETIDINE
1-BENZHYDRYLAZETIDIN-3-YL METHANESULFONATE
1-DIPHENYLMETHYL-3-AZETIDINYL METHANESULFONATE
1-(DIPHENYLMETHYL)-3-(METHANESULFONYLOXY)AZETIDINE
BUTTPARK 37\04-14
1-(diphenylmethyl)-3-(methanesulfonyloxy)azetinide
1-Diphenylmethyl-3-azetidinyl Methanethiosulfonate
1-Benzhydryl-3-methanesulphonyloxyazetidine
1-BENZHYDRYL-3-METHANESULFONATOAZETIDINE 98%
Methanesulfonic acid 1-benzhydryl-azetidin-3-yl ester
1-(Diphenylmethyl)-3-(mesyloxy)azetidine
1-(Diphenylmethyl)-3-[(methylsulfonyl)oxy]azetidine
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

18621-17-5

124-63-0

33301-41-6
在氮?dú)獗Wo(hù)下,將1-二苯甲基-3-羥基氮雜環(huán)丁烷(15.0 g,62.7 mmol)溶解于無(wú)水二氯甲烷(1 mL)中,冷卻至0℃(冰水?。?。向此溶液中加入干燥的三乙胺(25 mL,94.0 mmol)。隨后,通過(guò)加壓均流加料漏斗緩慢滴加甲基磺酰氯(5.8 mL,75.2 mmol)的無(wú)水二氯甲烷(50 mL)溶液。滴加完畢后,移除冷卻浴,繼續(xù)攪拌反應(yīng)混合物2小時(shí)。反應(yīng)完成后,用去離子水(70 mL)淬滅反應(yīng),分離有機(jī)層和水層。水層用二氯甲烷(2×100 mL)萃取。合并有機(jī)層,用無(wú)水硫酸鎂干燥,過(guò)濾后濃縮,得到澄清無(wú)色油狀物。向此油狀物中加入己烷(100 mL),促使產(chǎn)物固化。通過(guò)真空過(guò)濾收集固體產(chǎn)物,并在高真空下干燥,得到19.7 g(收率100%)的1-二苯甲基-3-甲烷磺酸氮雜環(huán)丁烷(12),為無(wú)色固體。
參考文獻(xiàn):
[1] Patent: US2005/54697, 2005, A1. Location in patent: Page/Page column 78
[2] Bioorganic and Medicinal Chemistry Letters, 2009, vol. 19, # 4, p. 1084 - 1088
[3] Patent: WO2011/61214, 2011, A1. Location in patent: Page/Page column 85-86
[4] Patent: US2014/288045, 2014, A1. Location in patent: Paragraph 0605
[5] Patent: WO2016/44772, 2016, A1. Location in patent: Paragraph 319