HRID451800

反应详情

EQUATION

反应方程式

HRID 451800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1,2,3,6-tetrahydropyridine (5.0 g, 60.15 mmol) and triethylamine (16.77 mL, 2 equiv) in CH2Cl2 (50 mL) was cooled to 0° C. (ice-water bath) followed by slow addition of benzyl chloroformate (9.7 mL, 1.1 equiv). After 30 min, the reaction mixture was allowed to warm slowly to rt and stirred for 4 h. The mixture was diluted with ether (300 mL), washed with 5% aq HCl (2×50 mL), satd aq NaHCO3 (40 mL) and brine (40 mL), and dried over Na2SO4. After concentration, benzyl 5,6-dihydropyridine-1(2H)-carboxylate (9.93 g, 78% yield) was left.

WORKUP

后处理

  1. washwashed with 5% aq HCl (2×50 mL)
  2. dry with materialdried over Na2SO4