反応 #531857

反応方程式

4-(3-adamantan-1-yl-ureido)butyric acid

K2CO3

iodomethane

→

883

収率 95.0%

4-(3-Adamantan-1-yl-ureido) butyric Acid Methyl Ester

収率 95.0%

溶媒

DMF

反応条件

後処理

1. 1
   抽出Then the product was extracted with ether (20 mL)
2. 2
   洗浄the ether was washed with 1 N NaOH aqueous solution (20 mL) and brine (20 mL)
3. 3
   乾燥dried over Na2SO4
4. 4
   その他evaporated

実験手順

A mixture of 4-(3-adamantan-1-yl-ureido)butyric acid 822 (0.15 g, 0.54 mmol), K2CO3 (0.09 g, 0.64 mmol), and iodomethane (0.04 mL, 0.59 mmol) in DMF (20 mL) was stirred at room temperature for 20 h. Then the product was extracted with ether (20 mL), and the ether was washed with 1 N NaOH aqueous solution (20 mL) and brine (20 mL), dried over Na2SO4, and evaporated to afford 0.15 g (95%) of 883: 1H NMR (CDCl3) 1.66-1.68 (6H, m), 1.81 (2H, quint, J=6.9 Hz), 1.94-1.97 (6H, m), 2.05-2.07 (3H, m), 2.37 (2H, t, J=6.9 Hz), 3.16 (2H, q, J=6.9 Hz), 3.68 (3H, s), 4.09 (1H, s), 4.25 (1H, s); LC-MS (ESI) m/z calcd for C16H26N2O3 [M+H]+ 295.19. found [M+H]+ 295.24; mp 114 C. Anal. (C16H26N2O3) C, H, N.

出典