HRID750002
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 55 °C
PROCEDURE
实验过程
To the product from step 1 (55 mg, 0.127 mmol) in 1,4-dioxane (2 mL) was added 12N HCl (1.7 mL) and the resulting mixture was stirred at 55° C. for 5 h. The solvent was removed in vacuo to obtain the product as a solid. The oil was triturated with diethyl ether (4 mL) to obtain the title product as a white solid (27 mg, 52%): MS; m/z 374 (M−H): LCMS (UV) 94%; 1H NMR (400 MHz, DMSO-d6) δ 1.49-1.54 (m, 1H), 1.74-1.83 (m, 4H), 1.93-1.96 (m, 1H), 3.30-3.36 (m, 2H), 3.44-3.47 (m, 1H), 3.82-3.84 (m, 1H), 4.02-4.06 (m, 1H), 4.17-4.20 (m, 2H), 4.29-4.33 (dd, 1H J1=6.8 Hz, J2=10.8 Hz), 6.93-6.95 (m, 2H) 6.95-6.98 (m, 2H), 7.00-7.07 (m, 2H), 7.39-7.41 (m, 2H).
WORKUP
后处理
- customThe solvent was removed in vacuo