Acetic Acid → HCID 178481859, compound

Temperature

10 °C

92.1 g (0.5 mole) of ethyl 4,4,4-trifluoroacetoacetate was dissolved in 60.1 g (1.0 mole) of acetic acid. The solution was cooled to 10° C. or lower with stirring. Thereto was dropwise added, in 1 hour, 65.8 g (0.5 mole) of a 35% aqueous methylhydrazine solution. After the dropwise addition, the mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours to give rise to a reaction. After the reaction, the mixture was cooled to room temperature. Thereto were added 150 ml of toluene, 600 ml of water and 48 g (1.2 moles) of sodium hydroxide. After phase separation, 154 g (1.5 moles) of 35% hydrochloric acid was added to the aqueous layer. The resulting crystals were collected by filtration, washed with 50 ml of water twice, and dried in a hot-air drier, to obtain 71.8 g (yield: 86.5%) of a title compound as light yellow crystals.

1. additionThereto was dropwise added, in 1 hour
2. additionAfter the dropwise addition
3. stirringthe mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours
4. customto give rise
5. customto a reaction
6. customAfter the reaction
7. temperaturethe mixture was cooled to room temperature
8. additionwas added to the aqueous layer
9. filtrationThe resulting crystals were collected by filtration
10. washwashed with 50 ml of water twice
11. customdried in a hot-air drier,

ORD record

ord-ab2bb8514dfb4e2d97c1955190d7b886

Source dataset

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07812175B2