HRID2353226

反应详情

EQUATION

反应方程式

HRID 2353226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound from step 2 (554 mg, 2.11 mmol) and iodobenzene (430 mg, 2.11 mmol) were dissolved in toluene (15 ml) and the following reagents were added: Pd2(dba)3 (58 mg, 0.063 mmol), PtBu3 (128 mg. 0.63 mmol) and NaO-t-Bu (202 mg, 2.11 mmol). The reaction mixture was stirred at ambient temperature overnight and then filtered. The filtrate was loaded onto a silica gel column and eluted with 1% MeOH in CH2Cl2 to yield the title compound as a yellow solid (85 mg, 11.9%): MS (ESI) m/z 340 (M+H); 1H NMR (400 MHz, CDCl3) δ 2.56 (t, J=7.2 Hz, 2H), 2.64 (t, J=4.8 Hz, 4H), 2.77 (t, J=7.2 Hz, 2H), 3.13 (br, 4H), 3.69 (s, 3H), 6.82-7.21 (m, 9H).

WORKUP

后处理

  1. additionthe following reagents were added
  2. filtrationfiltered
  3. washeluted with 1% MeOH in CH2Cl2