反应详情

温度

80 °C

tert-Butyl-3-methylpiperazine carboxylate (1.49 g, 7.45 mmol) and paraformaldehyde (1.12 g, 37.2 mmol) were dissolved in a mixture of MeOH and acetic acid (5:1) on molecular sieves. NaBCNH3 (1.88 g, 29.8 mmol) was added to the suspension at 25° C. The slurry was subsequently heated to 80° C. for 10 hr. Then the mixture was cooled, filtered, and concentrated. The residue was dissolved in dichloromethane and washed with saturated sodium bicarbonate. The organic solution was dried over Na2SO4, and concentrated to give a white oily (1.2 g, 90%). LC-MS (ESI) m/z: 215 (M+1)+.

1. additionNaBCNH3 (1.88 g, 29.8 mmol) was added to the suspension at 25° C
2. temperatureThen the mixture was cooled
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in dichloromethane
6. washwashed with saturated sodium bicarbonate
7. dry with materialThe organic solution was dried over Na2SO4
8. concentrationconcentrated
9. customto give a white oily (1.2 g, 90%)