HRID370376
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis refluxed for about 16 hours
- filtrationThen, the mixture is filtered
- concentrationfiltrate concentrated
- customThe concentrate is purified by prep