HRID551934

反应详情

EQUATION

反应方程式

HRID 551934 的结构方程式

PROCEDURE

实验过程

The title compound was prepared following procedure described in example 19, step b) from 2-[(4-butylphenyl)ethynyl]benzaldehyde (1.12 g, 4.28 mmol, intermediate which may be obtained according to methods disclosed in EP03103780.7) and n-hexylamine (Aldrich, 294 μl, 5.13 mmol). Purification of the crude product by flash chromatography on silicagel (DCM/MeOH/NH4OH 98/2/1) gave 174 mg (12%) of the title compound. HPLC, Rt: 4.39 min purity: 91.6%). LC/MS, M+(ESI): 348.4. 1HNMR (CDCl3) δ: 0.82 (t, J=6.8 Hz, 3H), 0.91 (t, J=7.3 Hz, 3H), 1.23-1.40 (m, 8H), 1.46-1.64 (m, 4H), 2.25 (m, 1H), 2.62 (t, J=7.5 Hz, 4H), 4.00 (s, 2H), 7.15 (d, J=8.3 Hz, 2H), 7.17-7.26 (m, 2H), 7.39 (m, 1H), 7.42 (d, J=8.3 Hz, 2H), 7.50 (dd, J=7.3, 1.7 Hz, 1H).

WORKUP

后处理

  1. customThe title compound was prepared following procedure
  2. customPurification of the crude product by flash chromatography on silicagel (DCM/MeOH/NH4OH 98/2/1)