反应详情

温度

110 °C

The compound from Example 1, Step 3 (0.16 g 0.45 mmol), cyclohexyl mercaptan (0.16 g, 1.35. mmol) and sodium hydride (60% dispersion in oil, 4.0 equiv, 0.032 g) were suspended in DMF (0.5 mL) in an N2 purged sealed tube and heated at 110° C. for 4hr. 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: 389 found: 389. 1H-NMR (CD3OD): 1.4-2.1 ppm (10H); 3.8 ppm (1H); 4.2 ppm (2H); 5.45 ppm (2H); 7.2-7.6 ppm (7H); 8.2 ppm (1H); 9.1 ppm (1H).

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