HRID489601

反应详情

EQUATION

反应方程式

HRID 489601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 0.2 g of 4-(3-Aminomethyl-phenyl)-1-tert-butoxycarbonyl-piperidine-4-carbonitrile in 15 ml of dichloromethane was added a few drops of triethylamine followed by a few drops of benzyl chloroformate. The mixture was stirred for 1 hour at room temperature and was poured into aqueous sodium carbonate and was extracted with dichloromethane. The organic layer was dried over magnesium sulfate and was filtered. The filtrate was evaporated and the residue was used directly in the next step without further purification: 1H-NMR (300 MHz, CDCl3)δ (TMS) 1.39-1.52 (m, 9H), 1.80-2.16(m, 4H), 3.08-3.42(m, 4H), 4.19-4.50(m, 2H), 5.08-5.13(d, 2H), 7.28-7.79(m, 9H), MS (ESI) m/e 450 (M+H)+.

WORKUP

后处理

  1. extractionwas extracted with dichloromethane
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationwas filtered
  4. customThe filtrate was evaporated
  5. customthe residue was used directly in the next step without further purification