N,N-Dimethyl-1,3-propanediamine → Lauramidopropyl Dimethylamine

Temperatur

0 °C

A 500 ml RB flask containing a solution of lauroyl chloride (19.38 g., 89 mM) in dry chloroform (200 ml) was cooled to 0° C. on an ice bath. A solution of N,N-dimethyl-1, 3-propanediamine (10.40 g., 51 mM) and triethylamine (9.40 g., 93 mM) in dry chloroform (25 ml) was added dropwise to the cold solution through an addition funnel, then allowed to warm to room temperature and stirred for 2 hours. The chloroform was removed under reduced pressure and the residue redissolved in an ethanol/water mixture (1:1) and neutralized with sodium bicarbonate, followed by extraction with chloroform (4×50 ml). The combined extracts were dried (MgSO4), concentrated, and the residue distilled under reduced pressure (bp 171° C., 10μ) to give 23.92 g. (68%) of the subject compound as an amber solid.

1. temperatureto warm to room temperature
2. customThe chloroform was removed under reduced pressure
3. dissolutionthe residue redissolved in an ethanol/water mixture (1:1)
4. extractionfollowed by extraction with chloroform (4×50 ml)
5. dry with materialThe combined extracts were dried (MgSO4)
6. concentrationconcentrated
7. distillationthe residue distilled under reduced pressure (bp 171° C., 10μ)
8. customto give 23.92 g

ORD-Eintrag

ord-9bbf9a6113d44d758b00f4dfd97ec540

Quelldatensatz

uspto-grants-1997_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05631005