Hydrochloric Acid → 4-Propylheptan-4-amine--hydrogen chloride (1/1)

Temperature

90 °C

Into a three-necked flask equipped with a mechanical stirrer, a dropping-funnel, a thermometer and a condenser, were introduced 200 ml of water and 90 ml of concentrated hydrochloric acid (d=1.19). The acid solution was heated to 90° C and then, under vigorous stirring, 105 g of 1,1-di-n-propyl-n-butylisocyanate, prepared as previously described, were slowly added. The operation of addition lasted one hour after which the reaction medium was heated for a further 4 hours at a temperature between about 95° and 100° C. The mixture was then cooled to about 0° C and the colourless crystals so obtained were filtered off dried by exposure to the air and then in a dessicator in the presence of potassium hydroxide. In this manner, 99 g of 1,1-di-n-propyl-n-butylamine hydrochloride were isolated in the form of a white crystalline powder.

1. customInto a three-necked flask equipped with a mechanical stirrer, a dropping-funnel
2. additionwere slowly added
3. additionThe operation of addition
4. temperatureafter which the reaction medium was heated for a further 4 hours at a temperature between about 95° and 100° C
5. temperatureThe mixture was then cooled to about 0° C
6. customthe colourless crystals so obtained
7. filtrationwere filtered off
8. customdried by exposure to the air

ORD record

ord-8431992b89134e4584ac35acea3f64b9

Source dataset

uspto-grants-1977_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04057644