HRID1059976

反应详情

EQUATION

反应方程式

HRID 1059976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 5-(4-methoxypyridin-2-yl)-2-methylaniline (200 mg), N,N′-bis(tert-butoxycarbonyl)thiourea (310 mg) and diisopropyl-ethylamine (0.374 ml) in dichloromethane (10 ml) was added 1-methyl-2-chloropyridinium iodide (310 mg), and the mixture was stirred for 2 hours. The mixture was diluted with dichloromethane, washed with water and brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 25 g, n-hexane:ethyl acetate=3:1) to give N,N′-bis(tert-butoxycarbonyl)-N″-(5-(4-methoxypyridin-2-yl)-2-methylphenyl)guanidine (357 mg).

WORKUP

后处理

  1. washwashed with water and brine
  2. dry with materialdried over magnesium sulfate
  3. customevaporated under reduced pressure
  4. customThe residue was purified by column chromatography (silica gel 25 g, n-hexane:ethyl acetate=3:1)