反应详情

温度

80 °C

Tert-butyl 2,2-dimethyl-5-(5-(trifluoromethyl)-6-(4-(trifluoromethyl)cyclohexyloxy)naphthalen-2-yl)-1,3-dioxan-5-ylcarbamate (1000.1 mg, 0.0016906 mol) (impure, assume 100% purity) was dissolved in methanol (30 mL, 0.73 mol), followed by 1 M of hydrogen chloride in water (30 mL, 0.030 mol). The reaction mixture was then heated at 80° C. for 2.5 hours. The solvent was removed under reduced pressure and the crude residue was treated with 4 N HCl in 1,4-dioxane. The solution was stirred for 1 hour and the solvent was then removed under reduced pressure. Ethyl ether was then added and the resulting solid was removed via filtration to give 815 mg of the desired product a white solid (64%). ESI-MS: 417 (M−16)+ 1H NMR (400 MHz, DMSO-d6) δ=8.21-7.97 (m, 3H), 7.82-7.61 (m, 2H), 5.57-5.41 (m, 4H), 5.10 (br. s., 0.61H), 4.98-4.88 (m, 0.32H), 3.97-3.72 (m, 1H), 2.15-1.91 (m, 2H), 1.82-1.08 (m, 6H)

1. customThe solvent was removed under reduced pressure
2. additionthe crude residue was treated with 4 N HCl in 1,4-dioxane
3. customthe solvent was then removed under reduced pressure
4. additionEthyl ether was then added
5. customthe resulting solid was removed via filtration