Ammonia → HCID 86733459, compound

3-Chloro-3-methyl-2-nitrosobutane (60 g.) was added portionwise to dry methanol (600 ml.) saturated with ammonia at 0°. The solution was left at room temperature for 5 hours then refluxed for 16 hours in the presence of a stream of dry ammonia. The mixture was evaporated to dryness in vacuo at room temperature and the residue extracted with hot dry benzene (900 ml.) followed by boiling secondary butanol (1300 ml.). The secondary butanol extract was evaporated in vacuo at room temperature to a thick slurry. This was cooled, filtered and dried in vacuo (56 g.) m.p. 190° (decomp).

1. customThe mixture was evaporated to dryness in vacuo at room temperature
2. extractionthe residue extracted with hot dry benzene (900 ml.)
3. extractionThe secondary butanol extract
4. customwas evaporated in vacuo at room temperature to a thick slurry
5. temperatureThis was cooled
6. filtrationfiltered
7. customdried in vacuo (56 g.) m.p. 190° (decomp)

ORD record

ord-64534538005446de9c175f727880b479

Source dataset

uspto-grants-1976_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03959278