HRID2273621

反应详情

EQUATION

反应方程式

HRID 2273621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of compound 10 (0.23 g, 0.45 mmol) in anhydrous dichloromethane (5 mL) was added, under argon, a 2.0 N hydrochloric acid solution in anhydrous ether (10 mL). The mixture was stirred at room temperature for 10 min and the solvent was evapored under vacuum. The residue was then suspended in anhydrous ether (10 mL) and the mixture was stirred, under argon, at room temperature for one night. The precipitate was collected by filtration to give compound 11 (0.24 g, 0.41 mmol) as a very hygroscopic beige solid. Yield 91%; mp 99-101° C. (dec.); IR (KBr) ν 1464, 1533, 1560, 1671, 2400-2700, 2800-3100, 3200-3400 cm−1; 1H NMR (200 MHz, DMSO-d6) δ 1.31 (t, 3H, J=7.0 Hz), 3.40 (m, 4H), 3.78 (m, 4H), 4.19 (m, 6H), 4.55 (t, 2H, J=3.5 Hz), 7.28 (dd, 1H, J=5.3, 7.7 Hz), 7.70 (m, 2H), 7.90 (d, 1H, J=8.8 Hz), 8.25 (dd, 1H, J=1.9, 8.8 Hz), 8.64 (d, 1H, J=1.8 Hz), 9.40 (m, 2H), 10.53 (se, 1H); ESI-MS m/z 509.9 [M+H]+; Anal. Calcd for C20H21O2IN5F, 2HCl, H2O: C, 40.02; H, 4.20; N, 11.67. Found: C, 40.40; H, 4.34; N, 11.28.

WORKUP

后处理

  1. stirringthe mixture was stirred, under argon, at room temperature for one night
  2. filtrationThe precipitate was collected by filtration