HRID30254

反应详情

EQUATION

反应方程式

HRID 30254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product of step c) (20.9 mg, 0.07 mmol) in CH2Cl2 (330 μl) was treated with iodotrimethylsilane (19.8 mg, 0.099 mmol) at 50° C. for 16 hours. The solvent was evaporated in vacuo leaving a brown residue that was dissolved in MeOH and a portion purified by preparative LC/MS to give the title compound. 1H NMR (300 MHz, CDCl3, ppm) 2.76-2.81 (m, 1H); 2.95-3.03 (m, 1H); 3.12-3.22 (m, 2H); 3.44-3.61 (m, 3H); 3.81-3.85 (m, 1H); 6.78 (s, 1H); 9.20-9.4 (br s, 2H); MS calculated for C9H10BrNS+H 244, observed 244, 246.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. customleaving a brown residue that
  3. customa portion purified by preparative LC/MS