反应 #2322556

ord-446df5ba0a354621ab21e11178288f2c

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他at 40° C.
  2. 2
    其他for 4 d
  3. 3
    其他After aqueous work-up and purification by RP chromatography the pure material (0.77 g)
  4. 4
    温度at reflux

实验过程

Analogously to general procedure (I) N-(3,3-dimethyl-6-nitro-2-oxo-2,3-dihydro-1H-indol-5-yl)-acetamide (1 g) is alkylated using 1-chloro-2-ethylsulfanyl-ethane (0.5 ml; 3.83 mmol) and K2CO3 (0.54 g; 3.83 mmol) at 40° C. for 4 d. After aqueous work-up and purification by RP chromatography the pure material (0.77 g) is de-acetylated in MeOH (35 ml) using DBU (0.3 ml) at reflux. After aqueous work-up 5-amino-1-(2-ethylsulfanyl-ethyl)-3,3-dimethyl-6-nitro-1,3-dihydro-indol-2-one (0.65 g) is obtained and used without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07714010B2uspto-grants-2010_05