HRID38900
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 [(2S)-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.5 g, 1.1 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, first with (DCM/MeOH) as eluent and then (EtOAc/MeOH) as eluent. Yield: 0.2 g, 72%. The amine was converted to the hydrochloric acid salt and crystallized from EtOH/Et2O. M.p. 226° C. MS m/z (rel. intensity, 70 eV) 311 (M+, 1), 310 (M+, 1), 99 (7), 98 (bp), 79 (2), 55 (4). [α]=+62° (MeOH).
WORKUP
后处理
- customPurification on SCX-3 column (TEA/MeOH)
- customcrystallized from EtOH/Et2O
- custom[α]=+62° (MeOH)