22680-44-0
22680-44-0 結(jié)構(gòu)式
基本信息
噻氯匹定雜質(zhì)C
(2-氯苯基)甲胺鹽酸鹽
(2-氯苯基)甲酰胺鹽酸鹽
3-氯吡嗪-2-甲胺鹽酸鹽
3-氯吡嗪-2-甲胺一鹽酸鹽
鹽酸噻氯匹啶EP雜質(zhì)C鹽酸鹽
鹽酸噻氯匹定雜質(zhì)C(EP) 標(biāo)準(zhǔn)品
(2-Chlorophenyl)methanamine Hydroch
(3-Chloropyrazin-2-yl)-MethanaMine HCl
(2-Chlorophenyl)MethanaMine hydrochloride
3-Chloropyrazin-2-methanamine hydrochloride
2-Aminomethyl-3-chloropyrazine hydrochloride
Ticlopidine Hydrochloride Impurity C as Hydrochloride
Ticlopidine Hydrochloride EP Impurity C as Hydrochloride
制備方法
873-32-5
22680-44-0
一般步驟:在手套箱中,向裝有磁力攪拌棒的火焰干燥的GLC小瓶中依次加入[3a] + [BArF4](1.0 mol%)和Me2PhSiH(2a)(2.1或5.0當(dāng)量)。對于固體原料,將指定的腈加入手套箱中;對于液體原料,則通過手套箱外的微量注射器加入。將反應(yīng)混合物在室溫下攪拌反應(yīng)指定時間。反應(yīng)完成后,用含有4% Et3N的環(huán)己烷與叔丁基甲基醚(90:10,0.5 mL)混合液淬滅反應(yīng)。將所得溶液通過涂有少量硅膠的硅藻土墊過濾,使用相同比例的環(huán)己烷與叔丁基甲基醚(含4% Et3N,3-4 mL)作為洗脫液。減壓濃縮除去溶劑,將殘余物溶于Et2O(1 mL)中,隨后加入2M HCl的Et2O溶液(1.0 mL,2.0 mmol,10當(dāng)量)。將生成的懸浮液攪拌1小時后過濾,得到(2-氯苯基)甲酰胺鹽酸鹽,為白色至黃色固體。
參考文獻(xiàn):
[1] Synlett, 2017, vol. 28, # 18, p. 2411 - 2414
[2] Journal of the American Chemical Society, 2016, vol. 138, # 28, p. 8781 - 8788
[3] Journal of the American Chemical Society, 2016, vol. 138, # 28, p. 8809 - 8814
[4] Journal of Organic Chemistry, 2015, vol. 80, # 14, p. 7281 - 7287
[5] Catalysis Science and Technology, 2018, vol. 8, # 2, p. 499 - 507