Reaktionsgleichung
[CH:1]([OH:3])=[O:2].C(OC(=O)C)(=O)C.[CH:11]([NH:13][C:14]([CH3:19])([CH3:18])[CH2:15][CH2:16]O)=[O:12]>>[CH:1]([O:3][CH2:16][CH2:15][C:14]([NH:13][CH:11]=[O:12])([CH3:19])[CH3:18])=[O:2]Komponenten
4
Versuchsvorschrift
Formic acid (6.90 g, 0.15 mol) was added to acetic anhydride (15.30 g, 0.15 mol) and warmed to 45°-50° C. for one hour on a water bath. The resulting solution was cooled to below 0° C. in an ice/acetone bath. 3-Formamido-3-methyl-1-butanol (13.10 g, 0.10 mol) was added and the solution allowed to slowly warm to room temperature with stirring (16 hours). The solution was distilled under vacuum (1 Torr, 105°-110° C.) to yield 12.43 g (78%).
Aufarbeitung
- temperaturewarmed to 45°-50° C. for one hour on a water bath
- temperatureThe resulting solution was cooled to below 0° C. in an ice/acetone bath
- distillationThe solution was distilled under vacuum (1 Torr, 105°-110° C.)
- customto yield 12.43 g (78%)
Quellen und Nachweise
- ORD-Eintrag
- ord-56fae769693448d78758605fb23f1d64
- Quelldatensatz
- uspto-grants-1991_01
- Patentnummer
- US04988827
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