HRID18096
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
Benzoyl chloride (1.2 ml) was added dropwise to sodium thiocyanate (0.90 g) in acetone (50 ml). When the addition was complete the mixture was refluxed for 15 minutes, cooled to room temperature and (RS) 2-aminomethyl-piperidine-1-carboxylic acid tert butyl ester (2.0 g) in acetone (5 ml) added. The mixture was refluxed for 2 hours, cooled to room temperature and solvent removed at reduced pressure. The residue was column chromatographed (silica gel, 0-10% (9:1 methanol/ammonia) in dichloromethane eluant) to give the title product (1.95 g).
WORKUP
后处理
- additionWhen the addition
- temperaturewas refluxed for 15 minutes
- temperatureThe mixture was refluxed for 2 hours
- temperaturecooled to room temperature
- customsolvent removed at reduced pressure
- customchromatographed (silica gel, 0-10% (9:1 methanol/ammonia) in dichloromethane eluant)