HRID38960
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-fluoro-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.2 g, 0.5 mmol), propan-1-amine (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 (isooctane/EtOAc/MeOH). Yield: 0.12 g, 79%. The amine was converted to the hydrochloric acid salt and crystallized from MeOH/Et2O. M.p. 192° C. MS m/z (rel. intensity, 70 eV) 303 (M+, 2), 73 (5), 72 (bp), 70 (11), 69 (7), 63 (5). [α]=−64° (MeOH).
WORKUP
后处理
- customPurification on SCX-3 column (TEA/MeOH)
- customcrystallized from MeOH/Et2O
- custom[α]=−64° (MeOH)