Sulfuric Acid → HCID 12426735, compound

Into a 150 ml flask, provided with a reflux condenser, were placed 14.6 g of monosec.butylamine dissolved in 15.5 ml of C2H5OH. Added thereto was 30 g of 2-bromo-pentane. This mass was then boiled to reflux temperature for 10-12 hours and thereafter cooled down and neutralized with dilute H2SO4. The whole was then evaporated to dryness. The residue thus obtained was treated with an excess of a 15% NaOH solution and extracted with 3 successive portions of ethyl ether. The ether extracts were then combined and washed with H2O, dried or anhydrous Na2SO4, filtered and the ether removed by evaporation. The residue was distilled under atmospheric pressure and the fraction was gathered which passed over at 160° - 161°C. 15.75 g of N-sec.butyl,N-sec.amylamine were obtained thereby. The picrate shows a melting point of from 61°-63°C (crystals from petroleum ether). The analysis of the picrate gave: calculated C = 48.58%, found C = 48.22%; calculated H = 6.50%, found H = 6.4%.

1. customInto a 150 ml flask, provided with a reflux condenser
2. additionAdded
3. temperatureto reflux temperature for 10-12 hours
4. temperaturecooled down
5. customThe whole was then evaporated to dryness
6. customThe residue thus obtained
7. extractionextracted with 3 successive portions of ethyl ether
8. washwashed with H2O
9. customdried
10. filtrationanhydrous Na2SO4, filtered
11. customthe ether removed by evaporation
12. distillationThe residue was distilled under atmospheric pressure
13. custompassed over at 160° - 161°C

ORD record

ord-407655eb12bc47b18010058dc8dd2293

Source dataset

uspto-grants-1976_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03982931