HRID459263

反应详情

EQUATION

反应方程式

HRID 459263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-(4-hydroxyphenyl)-2-phenoxypropanoic acid methyl ester (0.055 g, 0.18 mmol) with 1-(3-bromopropoxy)-4-phenoxybenzene (Step A) (0.055 g, 0.18 mmol) and potassium tert-butoxide (0.020 g, 0.18 mmol) were stirred in DMF (5 mL) overnight. The mixture reaction concentrated in vacuo with toluene (2 times), reconstituted in Ethyl acetate and washed with water (3 times) and brine, dryed (Na2SO4) and concentrated to afford a crude product that was purified by chromatographied in silicagel (hexanes/Ethyl acetate, 3:1) to give 0.022 g of the title compound (23%). 1H-NMR (200.15 MHz, CDCl3): δ 7.34–7.15 (m, 6H), 7.07–6.71 (m, 12H), 4.80–4.68 (m, 1H), 4.13 (t, 4H, J=15.1), 3.71 (s, 3H), 3.20–3.15 (m, 2H), 2.30–2.18 (q, 2H).

WORKUP

后处理

  1. customThe mixture reaction
  2. concentrationconcentrated in vacuo with toluene (2 times)
  3. washwashed with water (3 times) and brine
  4. concentrationconcentrated
  5. customto afford a crude product that
  6. customwas purified by chromatographied in silicagel (hexanes/Ethyl acetate, 3:1)