Hydrochloric Acid → HCID 20558300, compound

Temperature

70 °C

To 100 g of 2-ethylhexanoic acid (0.693 moles) was added 247.5 g of thionyl chloride (2.080 moles) over 30 minutes and then the solution was heated at 70° C. for 2 hours. To the cooled solution was added 185.2 g of N-chloro succinimide (1.387 moles), 165.0 g of thionyl chloride (1.387 moles) and 2.0 ml of concentrated HCl. The mixture was heated at 80° C. for 2 hours, after which time there was no more apparent Cl2 gas being given off. The mixture was cooled and filtered. The filtrate was distilled at atmospheric pressure to remove the SOCl2 and then distilled to give a major fraction at 95°-105° C. (20 mm) weighing 28.00 g. Purity was determined by GLC analysis. Purity (area %) was 85.7%; yield was 17.6%. The product had a satisfactory IR, and the NMR showed no detectable extra chlorination.

1. temperatureThe mixture was heated at 80° C. for 2 hours
2. temperatureThe mixture was cooled
3. filtrationfiltered
4. distillationThe filtrate was distilled at atmospheric pressure
5. customto remove the SOCl2
6. distillationdistilled
7. customto give a major fraction at 95°-105° C. (20 mm)

ORD record

ord-0d5f40d6905a49859c594ff9d7fbc2c2

Source dataset

uspto-grants-1981_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04307217