反应详情

温度

110 °C

The compound from Example 1 Step 3 (0.11 g 0.20 mmol), m-cresol (0.064 g, 0.59 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 24 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: 380.4 found: 381.0. 2 1H-NMR (CD3OD): 2.4 ppm (s, 3H); 4.2 ppm (s, 2H); 5.4 ppm (s, 2H); 6.8-7.6 ppm (11H); 7.9 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