反应详情

Methyl 5-[(4-chlorophenyl)(methylimino)methyl]-1,4-dimethyl-1H-pyrrole-2-acetate perchlorate (1.5 g, 3.6 mmole) was treated with saturated aqueous sodium bicarbonate and extracted with chloroform (50 ml). The organic phase was dried over magnesium sulfate, filtered and concentrated. The residue was treated with dimethyl sulfate (0.62 g, 4.9 mmole) and heated at ~40° C. for one hour. The viscous reaction mixture was dissolved in methanol (10 ml) and treated with sodium acetate (2 g, 24 mmole) and water (2 ml) and heated at reflux overnight. The reaction was cooled and diluted with water (5 ml). The crystalline solid was isolated by filtration, washed with water, air dried, and recrystallized from methanol (10 ml) to yield 0.71 g (65%) of the title compound as a tan solid, m.p. 125°-131° C.

1. extractionextracted with chloroform (50 ml)
2. dry with materialThe organic phase was dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. temperatureheated at ~40° C. for one hour
6. temperatureheated
7. temperatureat reflux overnight
8. temperatureThe reaction was cooled
9. customThe crystalline solid was isolated by filtration
10. washwashed with water, air
11. customdried
12. customrecrystallized from methanol (10 ml)