反应详情

温度

65 °C

The residue (N,N-dimethyl-8-phenyl-1,4-dioxaspiro-[4.5]decan-8-amine) was taken up in aqueous HCl at pH 1. It was stirred for 1 hour at 65° C. The batch was cooled and brought to pH 4 with NaOH solution. 2-MTHF (52 ml) was then added. The mixture was alkalised with NaOH at 15-25° C. to pH≧12. The organic phase was concentrated at 45° C. and at reduced pressure (<10 mbar). The residue was dissolved at 65° C. in twice the amount of isopropanol/H2O 60/40. The batch was stirred overnight at −10° C. The precipitate was suctioned off, subsequently washed with cold isopropanol/H2O and dried overnight in a drying cupboard (45° C., <100 mbar).

1. temperatureThe batch was cooled
2. concentrationThe organic phase was concentrated at 45° C. and at reduced pressure (<10 mbar)
3. dissolutionThe residue was dissolved at 65° C. in twice the amount of isopropanol/H2O 60/40
4. stirringThe batch was stirred overnight at −10° C
5. washsubsequently washed with cold isopropanol/H2O
6. customdried overnight in a drying cupboard (45° C., <100 mbar)