反应详情

温度

0 °C

A solution of 7.3 g (21.50 mmol) of 5-oxo-4-(3-piperidin-1-yl-propyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester was in 140 ml CH2Cl2, cooled to 0° C. and treated with 54 ml (215 mmol) of HCl solution (4 M dioxane), then warmed to RT. After 3 h, 40 ml of MeOH were added to dissolve the precipitation and stirring was continued over night. The solution was evaporated, dissolved in aq. sat. NaHCO3. solution, the water evaporated and the solid extracted with in CH2Cl2:MeOH 9:1. Concentration afforded the title compound 5.0 g (97%) as yellow oil. MS: 240.1 (MH+).

1. temperaturewarmed to RT
2. dissolutionto dissolve
3. customthe precipitation
4. waitwas continued over night
5. customThe solution was evaporated
6. dissolutiondissolved in aq. sat. NaHCO3
7. customsolution, the water evaporated
8. extractionthe solid extracted with in CH2Cl2:MeOH 9:1
9. concentrationConcentration