反应详情

温度

0 °C

Zinc powder (3.0 g) was added in portions to a solution of [1-(2-chloro-4-nitrophenyl)-pyrrolidin-3-yl]dimethylamine (1.9 g) in glacial acetic acid (50 mL) cooled to 0° C. After the addition was complete, the mixture was stirred at room temperature for 30 minutes and then insolubles were filtered off with suction. The filtrate was concentrated in a rotary evaporator, and the residue was partitioned between sodium hydroxide solution and ethyl acetate. The organic phase was dried over magnesium sulfate and concentrated. The product with the molecular weight of 239.75 (C12H18ClN3) was obtained in this way; MS (ESI): 240 (M+H+).

1. additionAfter the addition
2. filtrationinsolubles were filtered off with suction
3. concentrationThe filtrate was concentrated in a rotary evaporator
4. customthe residue was partitioned between sodium hydroxide solution and ethyl acetate
5. dry with materialThe organic phase was dried over magnesium sulfate
6. concentrationconcentrated
7. customThe product with the molecular weight of 239.75 (C12H18ClN3) was obtained in this way