HRID18096

反应详情

EQUATION

反应方程式

HRID 18096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionWhen the addition
  2. temperaturewas refluxed for 15 minutes
  3. temperatureThe mixture was refluxed for 2 hours
  4. temperaturecooled to room temperature
  5. customsolvent removed at reduced pressure
  6. customchromatographed (silica gel, 0-10% (9:1 methanol/ammonia) in dichloromethane eluant)