HRID2037495

反应详情

EQUATION

反应方程式

HRID 2037495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-[1-(4-bromo-phenyl)-ethylamino]-4-methyl-pentan-3-one (3.42 g, 0.01 mol) and K2CO3 (6.9 g, 0.05 mol) in dried CH2Cl2 (50 mL) was added chloroformate (1.41 g, 0.015 mol). The mixture was refluxed overnight. The solvent was removed to give the crude product, which was purified by column to give [1-(4-bromo-phenyl)-ethyl]-(4-methyl-3-oxo-pentyl)-carbamic acid methyl ester (2.8 g, 79%). 1H NMR (CDCl3): 1.01 (m, 6H), 1.48 (m, 3H), 2.25-2.47 (m, 2H), 2.62 (m, 1H), 3.24 (m, 2H), 5.46 (s, 1H), 7.17 (m, 2H), 7.45 (m, 2H).

WORKUP

后处理

  1. temperatureThe mixture was refluxed overnight
  2. customThe solvent was removed
  3. customto give the crude product, which
  4. customwas purified by column