HRID1072623

反应详情

EQUATION

反应方程式

HRID 1072623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The 7-nitrogramine salt (2.0 g, 5.8 mmol) is suspended in a mixture of 2-nitropropane (9.5 mL) and methanol (9.5 mL). Dimethylsulfate (1.09 mL, 11.5 mmol) is added dropwise via syringe, and the resulting yellow solution is stirred at room temperature for 5 minutes. Sodium methoxide (0.62 g, 11.5 mmol) is then added in one portion, and the mixture is stirred overnight at room temperature. The reaction is quenched by addition of saturated NH4Cl solution and ethyl acetate. The aqueous layer is extracted with ethyl acetate, and the combined organic layers are washed with brine, and dried over Na2SO4 to give 1.0 g of 3-(2-nitro-2-methylpropyl)-7-nitroindole (69%).

WORKUP

后处理

  1. stirringthe mixture is stirred overnight at room temperature
  2. customThe reaction is quenched by addition of saturated NH4Cl solution and ethyl acetate
  3. extractionThe aqueous layer is extracted with ethyl acetate
  4. washthe combined organic layers are washed with brine
  5. dry with materialdried over Na2SO4