Formic Acid → HCID 20512078, Verbindung

Reaktionsgleichung

[CH2:1]([N:4]([CH2:17][CH:18]=[CH2:19])[C:5]([CH:7]1[CH2:12][C:11]([CH3:14])([CH3:13])[NH:10][C:9]([CH3:16])([CH3:15])[CH2:8]1)=[O:6])[CH:2]=[CH2:3].[CH:20](O)=O.[OH-].[Na+]>C=O>[CH2:17]([N:4]([CH2:1][CH:2]=[CH2:3])[C:5]([CH:7]1[CH2:8][C:9]([CH3:16])([CH3:15])[N:10]([CH3:20])[C:11]([CH3:13])([CH3:14])[CH2:12]1)=[O:6])[CH:18]=[CH2:19]

Komponenten

Versuchsvorschrift

4-[(Diallylamino)carbonyl]-2,2,6,6-tetramethylpiperidine (58.0 grams; 0.219 mole) is slurried in 37% formaldehyde (98.6 mls) at room temperature and 95% formic acid (17.4 mls) is added thereto. The mixture is heated at reflux for 18 hours and the resulting two-phase reaction mixture is adjusted to pH 11-12 by adding 50% sodium hydroxide. The mixture is extracted with dichloromethane and the organic extracts are combined and evaporated to obtain a clear liquid which on distillation affords 58.3 grams of the desired product which boils at 118°-125° C. at 0.10-0.15 mm of mercury.