HRID38958
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 [(2R)-5-chloro-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.49 g, 1.1 mmol), piperidine (1 ml, 10.1 mmol) and MeOH (2 ml) was heated under microwave radiation at 120° C. for 25 min. Purification on SCX-3 column (TEA/MeOH) and by flash column chromatography (MeOH/EtOAc) gave the title compound (0.31 g). The amine was converted to the hydrochloric acid salt and crystallized from MeOH/Et20 (0.25 g). MS m/z (rel. intensity, 70 eV) 345 (M+, 0.5), 124 (3), 99 (7), 98 (bp), 96 (2), 55 (4) [α]=−60° (MeOH).
WORKUP
后处理
- customPurification on SCX-3 column (TEA/MeOH)