2-Chloro-3-nitropyridine → HCID 11147794, compound

A mixture of 18.3 g (115 mmol) of 2-chloro-3-nitropyridine and 300 ml of N-methylmorpholine was hydrogenated at room temperature and a hydrogen pressure of approximately 1.1 bar in the presence of 3 g of 5% platinum/charcoal (55.5% of water [Degussa]). After approximately 1.5 hours, the hydrogen uptake had ceased. The catalyst was removed by filtration through kieselguhr. The filtrate obtained was freed from solvent at approximately 45° C. under reduced pressure. Any remaining N-methylmorpholine was distilled off with 200 ml of Solvesso (Esso) under reduced pressure using a 20 cm column. The crystallizate which remained was taken up in 200 ml of n-hexane, filtered off with suction and washed with n-hexane. 15.9 g (96%) of the title compound were obtained as brown crystals.

1. customwas hydrogenated at room temperature
2. customThe catalyst was removed by filtration through kieselguhr
3. customThe filtrate obtained
4. customwas freed from solvent at approximately 45° C. under reduced pressure
5. distillationAny remaining N-methylmorpholine was distilled off with 200 ml of Solvesso (Esso) under reduced pressure
6. filtrationfiltered off with suction
7. washwashed with n-hexane

ORD record

ord-6cb5634e6a21464793ffdff85eceedb5

Source dataset

uspto-grants-1999_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05977146