反应详情

温度

110 °C

Intermediate 83 (7 g, 23.87 mmol), pyrrolidin-2-one (4.06 g, 47.74 mmol), CuI (909 mg, 4.77 mmol), N,N′-dimethylethylene diamine (10.28 ml, 95.49 mmol) and K2CO3 (7.25 g, 52.52 mmol) were suspended in toluene (10 ml) under N2 and heated to 110° C. for 16 h. After cooling to RT the reaction mixture was quenched by the addition of 100 ml water and extracted with ethyl acetate (three times). The organic layers were combined and washed with water and sat. aq NaCl-solution, dried with Na2SO4, filtered and evaporated to dryness, and purified by silica gel chromatography.

1. temperatureAfter cooling to RT the reaction mixture
2. customwas quenched by the addition of 100 ml water
3. extractionextracted with ethyl acetate (three times)
4. washwashed with water and sat. aq NaCl-solution
5. dry with materialdried with Na2SO4
6. filtrationfiltered
7. customevaporated to dryness
8. custompurified by silica gel chromatography