HRID1004205

反应详情

EQUATION

反应方程式

HRID 1004205 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.7 g (3.61 mmol) of 3-[1-(2,2-dimethyl-propionyl)-1H-indol-3-yl]-4-(1-methyl-6-nitro-1H-indol-3-yl)-pyrrole-2,5-dione (4) from Step E above in 60 ml of methanol was treated with 5.6 ml (8.96 mmol) of a 1.6 molar solution of NaOCH3 in methanol. The reaction was stirred at room temperature for 1 hour, poured in 2N-HCl/ice and extracted with ethyl acetate. The organic extracts were dried on anhydrous MgSO4 and concentrated to yield, after chromatographic purification, 394.7 mg (28%) of 3-(1H-indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-pyrrole-2,5-dione (I) as a red solid mp>280° C. MS: (M+), m/z 386.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic extracts were dried on anhydrous MgSO4
  3. concentrationconcentrated
  4. customto yield
  5. customafter chromatographic purification, 394.7 mg (28%) of 3-(1H-indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-pyrrole-2,5-dione (I) as a red solid mp>280° C