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) δ 7.31 (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