Adipoyl chloride → HCID 14800986, Verbindung

Temperatur

50 °C

In a three-necked round bottomed flask equipped with a reflux condenser, a glass gas inlet tube and a pressure equalizing dropping funnel was placed freshly distilled adipoyl chloride (2.60 ml, 17.50 mmol) dissolved in absolute chloroform (15 ml). The temperature was raised to ca. 50° C. and under a gentle stream of nitrogen through the solution, a solution of ethylidene bis(16-hydroxyhexadecanoate) (1.0 g, 1.75 mmol) in absolute chloroform (30 ml) was added dropwise and left at this temperature a further 3 hours after addition. The mixture was then cooled to room temperature and quickly transferred into a 50 ml round bottomed flask equipped for distillation under reduced pressure. Chloroform was first distilled off at normal pressure, then oil-pump vacuum was established and excess adipoyl chloride distilled off at ca. 75° C., 5 mbar pressure, leaving the residual title compound (1.56 g).

1. customIn a three-necked round bottomed flask equipped with a reflux condenser, a glass gas inlet tube
2. additionafter addition
3. temperatureThe mixture was then cooled to room temperature
4. customquickly transferred into a 50 ml round bottomed flask
5. customequipped for distillation under reduced pressure
6. distillationChloroform was first distilled off at normal pressure
7. distillationexcess adipoyl chloride distilled off at ca. 75° C.

ORD-Eintrag

ord-1fe368f8a7044d14ae02ac7bdc397392

Quelldatensatz

uspto-grants-1997_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05674468