Methane → HCID 178479081, compound

2-Aminopyridine (11.8 g.) was dissolved in 25 ml dichloroethane and the resulting clear solution chilled to 10°-15° C. Commercial 40% peracetic acid (20 g.) was slowly added over a 30-minute period with ice-cooling and stirring; the temperature was kept between 15°-20° C. After 1/2 hour stirring at 20°-30° C with very little cooling, the clear solution was allowed to react 15 hours at room temperature. Then was added 0.5 g. charcoal and the mixture kept at 70° C for 1 hour. The solution was filtered and the filtrate diluted with 100 ml dichloroethane. The clear solution was extracted twice with 30 ml of 20% hydrochloric acid. The acid extracts were washed with 30 ml dichloroethane and then evaporated under vacuum in a rotary evaporator to dryness to give 19.7 g. yellow crystals. Recrystallization from 1:1 ethanoltoluene mixture gave 13.7 g. nearly colorless crystals with m.p. 148° -152° C.

1. temperaturethe resulting clear solution chilled to 10°-15° C
2. temperaturecooling
3. customwas kept between 15°-20° C
4. stirringAfter 1/2 hour stirring at 20°-30° C with very little cooling
5. customto react 15 hours at room temperature
6. additionThen was added 0.5 g
7. filtrationThe solution was filtered
8. additionthe filtrate diluted with 100 ml dichloroethane
9. extractionThe clear solution was extracted twice with 30 ml of 20% hydrochloric acid
10. washThe acid extracts were washed with 30 ml dichloroethane
11. customevaporated under vacuum in a rotary evaporator to dryness
12. customto give 19.7 g
13. customRecrystallization from 1:1 ethanoltoluene mixture
14. customgave 13.7 g

ORD record

ord-554d12f91db647e3887b2d50b3bd4e10

Source dataset

uspto-grants-1978_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04080329