Triethylamine → HCID 12856025, Verbindung

A solution of 13.8 g. (200 mmole) of hydroxylamine hydrochloride and 27.8 ml. (200 mmole) of triethylamine in 500 ml. of methyl alcohol was cooled to a temperature of -5° C. and 30.2 g. (200 mmole) of methyl 3-pyridineacetate were added. The mixture was stirred for 6 hours at room temperature and then 10.8 g. (200 mmole) of sodium methylate were added causing a slight exotherm to occur. The reaction mixture was then stirred for 27.5 hours. The reaction mixture was filtered and the filtrate evaporated to dryness. The crude residue of product was sonicated with 50 ml. of chloroform and filtered. The insoluble crude product (25.10 g) was crystallized from 50 ml. of water. There were obtained 15.54 g. of product melting with decomposition at about 163° C. to about 165° C.

1. stirringThe reaction mixture was then stirred for 27.5 hours
2. filtrationThe reaction mixture was filtered
3. customthe filtrate evaporated to dryness
4. customThe crude residue of product was sonicated with 50 ml
5. filtrationof chloroform and filtered
6. customThe insoluble crude product (25.10 g) was crystallized from 50 ml
7. customThere were obtained 15.54 g
8. custommelting with decomposition at about 163° C. to about 165° C.

ORD-Eintrag

ord-d36d62e9adab45d58735bc2e1eff271b

Quelldatensatz

uspto-grants-1982_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04336253