反应详情

A solution of 2,4-dicarbethoxy-3 methylpyrrole (25) (2.44 g, 10.9 mmol), K2CO3 (9.9 g), and iodomethane (55 ml) in 750 ml acetone was refluxed at 50° C. for 15 hours. The solution was concentrated in vacuo, partitioned between 450 ml of dichloromethane and 600 ml of water. The aqueous layer was extracted with CH2Cl2 (2×500 ml), dried (sodium sulfate), and concentrated in vacuo to yield a brown oil that solidified upon standing at room temperature for several minutes and was used without further purification. (2.37 g. 91% yield). TLC (benzene) Rf 0.3; 1H NMR (CD2Cl2) δ7.31 (s, 1H), 4.23 (m, 4H), 3.84 (s, 3H), 2.54 (2, 3H), 1.33 (m, 6H).

1. concentrationThe solution was concentrated in vacuo
2. custompartitioned between 450 ml of dichloromethane and 600 ml of water
3. extractionThe aqueous layer was extracted with CH2Cl2 (2×500 ml)
4. dry with materialdried (sodium sulfate)
5. concentrationconcentrated in vacuo
6. customto yield a brown oil that
7. waitupon standing at room temperature for several minutes
8. customwas used without further purification