HRID1648166

反应详情

EQUATION

反应方程式

HRID 1648166 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 10 ml of methanol was dissolved 690 mg (2.25 mmole) of 1-(4-nitrobenzyl)-1,4,7,10-tetraazacyclododecane (prepared by the procedure of Example H). To the solution was added 350 mg of 10 percent palladium on carbon catalyst. Excess hydrogen was purged through the solution at 25° C. Within 45 minutes TLC indicated that the title product was prepared (Rf =0.33, Solvent System 3). Chromatographic purification of the formed titled product was conducted on 1 in.×16 in. flash silica column (Solvent System 3) and provided 480 mg (77 percent) of the title product as a pale yellow, clear oil.

WORKUP

后处理

  1. customprepared by the procedure of Example H)
  2. customExcess hydrogen was purged through the solution at 25° C
  3. customwas prepared (Rf =0.33, Solvent System 3)
  4. customChromatographic purification of the