反应详情

温度

105 °C

The compound from Step 3 (0.28 mmol, 0.164 g), 3-methyl thiophenol (0.85 mmol, 0.106 g) and triethylamine (3.59 mmol, 0.36 g) were placed in an N2 purged sealed tube. This was heated at 105° C. for 15 hr. The residue was dissolved in methanol and purified on a C18 preperative hplc column. Lyophilized from dioxane/HCl to provide the title compound. FAB-MS: calc: 396.4 found: 397.2 1H-NMR (CD3OD): 2.4 ppm (s, 3H); 4.2 ppm (s, 2H); 5.4 ppm (s, 2H); 7.2-7.6 ppm (1OH); 8.1 ppm (s, 1H); 9.1 ppm (s, 1H).

1. custompurged
2. customsealed tube
3. dissolutionThe residue was dissolved in methanol
4. custompurified on a C18 preperative hplc column