699-03-6

基本信息
4-溴-N-甲基芐胺
4-溴-N-甲基芐氨
N-甲基-4-溴芐胺
4-溴-N-甲基苯甲胺
1-(4-溴苯基)-N-甲基甲胺
Aids-107181
(4-BROMOBENZYL)METHY
874-73-7 (Hydrochloride)
(4-BROMOBENZYL)METHYLAMINE
4-BROMO-N-METHYLBENZYLAMINE
N-Methyl-4-bromobenzylamine
(4-Bromobenzyl)methylamine95%
(4-Bromobenzyl)Methylamine 95%
4-Bromo-N-methylbenzylamine 97%
物理化學(xué)性質(zhì)
制備方法

1122-91-4

74-89-5

699-03-6
N-甲基-4-溴芐胺的合成一般步驟:在高壓釜中,將4-溴苯甲醛(2.08 g,11.55 mmol)與2 M甲胺的甲醇溶液(25 mL,33.44 mmol)混合,于65℃下攪拌反應(yīng)4小時(shí)。反應(yīng)完成后,冷卻至室溫,分批加入硼氫化鈉(633 mg,16.72 mmol)。室溫下繼續(xù)攪拌30分鐘,隨后進(jìn)行真空濃縮。將殘余物溶解于乙酸乙酯(30 mL)中,有機(jī)層用飽和碳酸氫鈉水溶液洗滌。水相用幾滴1 N氫氧化鈉溶液調(diào)節(jié)至pH 13后,用乙酸乙酯萃取兩次。合并有機(jī)萃取物,用鹽水洗滌,無(wú)水硫酸鎂干燥,過(guò)濾后減壓濃縮,得到N-甲基-4-溴芐胺,為無(wú)色油狀物(2.04 g,收率91%),直接用于下一步反應(yīng)。LC-MS分析(分析條件A,Zorbax SB-AQ柱,酸性條件):保留時(shí)間t R = 0.61分鐘;[M + H]+ = 241.06(乙腈加合物)。
參考文獻(xiàn):
[1] Patent: WO2010/58353, 2010, A1. Location in patent: Page/Page column 77-78
[2] Patent: US2011/224210, 2011, A1. Location in patent: Page/Page column 54
[3] Phosphorus, Sulfur and Silicon and the Related Elements, 1993, vol. 78, # 1-4, p. 141 - 152
[4] Organic Letters, 2014, vol. 16, # 2, p. 358 - 361