HRID266674

反应详情

EQUATION

反应方程式

HRID 266674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-methoxycarbonylphenyl isocyanate (1.0 g, 5.6 mmol), N-methyl-2-iodoaniline, hydrochloride (1.6 g, 5.9 mmol) and N,N-diisopropylethylamine (1.1 mL, 6.3 mmol) in 100 mL of toluene was refluxed under N2 for 72 hours. The sample was concentrated, and partitioned between chloroform and 10% HCl. The chloroform was dried (MgSO4), filtered, concentrated and chromatographed (silica gel, methylene chloride) to give the title compound as a yellow solid, mp 144°-148° C.

WORKUP

后处理

  1. concentrationThe sample was concentrated
  2. custompartitioned between chloroform and 10% HCl
  3. dry with materialThe chloroform was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customchromatographed (silica gel, methylene chloride)