Azane;hydrate → HCID 86708824, compound

Temperature

50 °C

Under a nitrogen atmosphere, into a reaction vessel were charged 12.1 g (58.7 mmol) of (2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoic acid and 50 ml of water. A solution prepared by dissolving 12 ml of 25% ammonia water in 12 ml of water was dropped into this under cooling with ice over a period of 15 minutes. After completion of dropping, the solvent was distilled off under reduced pressure to obtain a residue to which 100 ml of tetrahydrofuran was added, and the mixture was stirred at 50° C. for 1 hour. Thereafter, the mixture was cooled down to room temperature, the deposited solid was isolated by filtration, and washed three times with 20 ml of tetrahydrofuran. The resultant solid was dried to obtain 11.1 g of ammonium (2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoate mono-hydrate as a gray-green powder. Yield: 79%.

1. customA solution prepared
2. additionwas dropped into
3. temperaturethis under cooling with ice over a period of 15 minutes
4. distillationthe solvent was distilled off under reduced pressure
5. customto obtain a residue to which 100 ml of tetrahydrofuran
6. additionwas added
7. temperatureThereafter, the mixture was cooled down to room temperature
8. customthe deposited solid was isolated by filtration
9. washwashed three times with 20 ml of tetrahydrofuran
10. customThe resultant solid was dried

ORD record

ord-f9f79648793d4d2bab2f1a0c1ccb7b89

Source dataset

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09365497B2