HRID38898
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A mixture of [7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.6 g, 1.5 mmol), piperidine (1 ml) and ACN (3 ml) was heated under microwave radiation at 120° C. for 20 min. Purification on SCX-3 column (TEA/MeOH) and by flash chromatography through a small plug of silica (DCM/MeOH, 5:95). Yield: 0.4 g, 85%. The amine was converted to the hydrochloric acid salt and crystallized from MeOH/Et2O. M.p. 248° C. MS m/z (rel. intensity, 70 eV) 311 (M+, 1), 310 (M+, 2), 207 (3), 99 (7), 98 (bp).
WORKUP
后处理
- customPurification on SCX-3 column (TEA/MeOH)
- customcrystallized from MeOH/Et2O