68947-43-3

基本信息
N-甲基-4-哌啶甲酸
N-甲基-4-羧酸哌啶
1-甲基哌啶-4-甲酸
1-甲基哌啶-4-羧酸
N-甲基-4-羧基-哌啶
1-甲基哌啶-4-甲酸 1G
1-甲基哌啶-4-甲酸, 98%+
1-甲基哌啶-4-甲酸 68947-43-3
4-Carboxy-1-methylpiperidine
1-METHYL-PIPERIDIN-4-CARBOXYLIC ACID
N-METHYLPIPERIDINE-4-CARBOXYLIC ACID
N-METHYL-4-PIPERIDINE CARBOXYLIC ACID
1-METHYL-PIPERIDINE-4-CARBOXYLIC ACID
1-methyl-Ppiperidine-4-carboxylic'acid
1-methylpiperidine-4-carboxylic acid(SALTDATA: HCl)
物理化學(xué)性質(zhì)
制備方法

498-94-2

50-00-0

68947-43-3
以4-哌啶甲酸(1 kg,7.74 mol)和甲醛(37%水溶液,720 g,8.87 mol,1.15 eq.)為原料,在10 L水中加入濕Pd/C催化劑(10%;55%糊劑,100 g),將混合物轉(zhuǎn)移至不銹鋼加氫反應(yīng)器中。用氫氣(3 bar)對反應(yīng)器進行加壓,反應(yīng)混合物在200-2500 rpm的攪拌速度下,于16-25℃反應(yīng)過夜。反應(yīng)完成后,過濾除去催化劑,濾液用500 mL水洗滌,隨后在真空下濃縮。殘余物通過乙醇(2×1 L)共沸蒸餾去除殘留水分。最后,將所得固體在50℃下真空干燥過夜,得到1-甲基哌啶-4-甲酸,為灰白色固體(1087 g,收率98.1%)。
參考文獻:
[1] Patent: WO2003/84949, 2003, A1. Location in patent: Page/Page column 45; 46
[2] Journal of Medicinal Chemistry, 2012, vol. 55, # 22, p. 10118 - 10129
[3] Patent: US6777428, 2004, B1. Location in patent: Page column 24
[4] Journal of Medicinal Chemistry, 1993, vol. 36, # 4, p. 449 - 459
[5] Patent: WO2008/62182, 2008, A1. Location in patent: Page/Page column 161-162