HRID370376

反应详情

EQUATION

反应方程式

HRID 370376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of N-methyl-N[2-nitro-5-(2-chloro-4-trifluoromethylphenoxy)phenyl]hydroxyamine (700 mg., 1.93 mm) K2CO3 (320 mg.), 1-bromo-3,3-dimethylbutan-2-one (520 mg.) and acetone (10 ml.) is refluxed for about 16 hours. Then, the mixture is filtered and filtrate concentrated. The concentrate is purified by prep. TLC using 20% ethyl acetate/hexane to give N-methyl-N-[2-nitro-5-(2-chloro-4-trifluoromethylphenoxy)phenyl]t-butylcarbonylmethoxyamine (IVA; R3 is H, n is one, and R4 is t-butyl).

WORKUP

后处理

  1. temperatureis refluxed for about 16 hours
  2. filtrationThen, the mixture is filtered
  3. concentrationfiltrate concentrated
  4. customThe concentrate is purified by prep