反应详情

9.4 mL (68 mmol) diphosphoryl chloride were slowly added dropwise to 10 g (62 mmol) 4-nitroindole and 11 g (68 mmol) methyl oxo-pyrrolidin-1-yl-acetate with stirring and while cooling with ice. The reaction mixture was heated to RT and stirred for 3 h at RT. Then first of all 10 mL MeOH were added dropwise at 0° C. and then saturated sodium hydrogen carbonate solution was added dropwise at 0° C. After repeated extraction with DCM the organic phase was dried and evaporated down to 100 mL. This residue was left to stand at RT and the precipitate formed was suction filtered, washed and dried in the air.

1. temperaturewhile cooling with ice
2. stirringstirred for 3 h at RT
3. extractionextraction with DCM the organic phase
4. customwas dried
5. customevaporated down to 100 mL
6. waitThis residue was left
7. customto stand at RT
8. customthe precipitate formed
9. filtrationfiltered
10. washwashed
11. customdried in the air