HRID2256050
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
PROCEDURE
实验过程
A solution of 1-benzyloxycarbonyl-4-(2-methylsulfinylphenyl)piperidine (1.66 g) in 8 mL of trifluoroacetic acid was heated to reflux for 45 minutes. At the end of this period, the reaction mixture was evaporated and the residue was treated with toluene. Upon evaporating the solvent, the residue was treated with an additional portion of toluene and the process was repeated. The final residue was dried under reduced pressure and purified by chromatography; elution with dichloromethane:methanol:triethylamine (19:1:1) afforded the named product (0.87 g); MS: 224; NMR: 1.6-2.4 (m, 4), 2.7 (two peaks, 3), 2.9-3.2 (m, 3), 3.3-3.5 (m, 2), 5.3-5.7 (br, 1), 7.4-7.5 (m, 3), 7.9-8.0 (m, 1).
WORKUP
后处理
- temperatureto reflux for 45 minutes
- customAt the end of this period, the reaction mixture was evaporated
- additionthe residue was treated with toluene
- customUpon evaporating the solvent
- additionthe residue was treated with an additional portion of toluene
- dry with materialThe final residue was dried under reduced pressure
- custompurified by chromatography
- washelution with dichloromethane:methanol:triethylamine (19:1:1)