Glycine → HCID 178446845, Verbindung

Temperatur

0 °C

A stirred suspension of glycine (18.77 g, 0.25 mol) in methanol (80 ml) and water (4.5 ml) was cooled to 0° C. and adjusted to pH 9.6 by adding 30 percent strength sodium hydroxide solution. Methyl pentanimidate (67.12 g of a 42.9 percent strength solution in toluene=0.25 mol) was added to this suspension over the course of 7 minutes. The reaction mixture was stirred for 5 hours at room temperature. Methanol and water were then distilled off at a reduced pressure of 30 mbar to 150 mbar. In total, 250 ml of toluene was added during this distillation. The mixture was then filtered, and the filter cake washed with toluene (75 ml) and dried. The yield of the title compound was 39.61 g (purity approximately 90 percent by H-NMR), 90 percent based on glycine.

1. distillationMethanol and water were then distilled off at a reduced pressure of 30 mbar to 150 mbar
2. additionIn total, 250 ml of toluene was added during this distillation
3. filtrationThe mixture was then filtered
4. washthe filter cake washed with toluene (75 ml)
5. customdried

ORD-Eintrag

ord-c36565a82d8044af8dacf26d6dc4dd59

Quelldatensatz

uspto-grants-1997_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05696272