反应详情

温度

90 °C

Hydrazine hydrate (1.92 g, 38.4 mmol) was added to a solution of methyl 3-formyl-4,5-dimethyl-1-[(1S,2S)-2-methylcyclopropylmethyl]pyrrole-2-carboxylate (7.96 g, 31.9 mmol) in acetic acid (38 ml) and the mixture was stirred at 90° C. for 1 hour. After this time, the reaction mixture was cooled to room temperature, poured into iced water and filtered. The crude crystals were washed with water and dissolved in a mixture of chloroform and methanol (9:1). The organic layer was separated, washed with saturated aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The solvent was removed in vacuo and to the residue was added a mixture of toluene and hexane. The precipitate was collected by filtration to afford the desired compound (7.02 g, 95.0%) as a pale yellowish white powder.

1. temperatureAfter this time, the reaction mixture was cooled to room temperature
2. filtrationfiltered
3. washThe crude crystals were washed with water
4. dissolutiondissolved in a mixture of chloroform and methanol (9:1)
5. customThe organic layer was separated
6. washwashed with saturated aqueous sodium chloride solution
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was removed in vacuo and to the residue
9. additionwas added
10. additiona mixture of toluene and hexane
11. filtrationThe precipitate was collected by filtration