反应详情

温度

65 °C

N-methyl-8-phenyl-1,4-dioxaspiro[4.5]decan-8-amine hydrochloride (15 g, 59 mmol) was taken up in water (37 ml) and 2-methyltetrahydrofuran (57 ml). The free base was released by adding NaOH aq (32%, to pH>12). The organic phase was concentrated at 45° C. at reduced pressure (<10 mbar). The residue was taken up in isopropanol (8 ml) and added dropwise to formic acid (7 ml, 0.19 mol) at up to 65° C. At 65° C., formaldehyde solution (5.8 g, 0.1 mol) was added swiftly and the batch was stirred overnight (approximately 16 h) at 65° C. The batch was concentrated at 80° C. and approximately 20 mbar. The remaining raw product was used in the next step without purification.

1. concentrationThe organic phase was concentrated at 45° C. at reduced pressure (<10 mbar)
2. concentrationThe batch was concentrated at 80° C.
3. customThe remaining raw product was used in the next step without purification