反应详情

温度

-60 °C

A solution of 3-(1H-indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-pyrrole-2,5-dione (250 mg, 0.65 mmol), prepared as described in U.S. Ser. No. 09/268,887, was dissolved in THF (15 ml) and cooled to −60° C. To this solution was added lithium bis(trimethylsilyl)amide (0.7 mmol, 0.7 ml, 1.0 M in THF), followed by oleyl chloride (Aldrich) (0.300 g, 1.0 mmol) in THF (5 ml). The resulting mixture was stirred at 0° C. for 1 hr. All solvent was evaporated and the crude material was pre-purified by silica gel chromatography. The resulting products were separated using silica gel chromatography using a gradient of ethyl acetate and hexane. This gave 310 mg of 3-(1H-Indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-1-octadec-9-enoyl-pyrrole-2,5-dione. (Yield 70 %)

1. customAll solvent was evaporated
2. customthe crude material was pre-purified by silica gel chromatography
3. customThe resulting products were separated