Hydrochloric Acid → HCID 178479629, compound

Ethyl 4,4,4-trifluoroacetoacetate (18.4 g (0.1 mol)) was dissolved in 20 mL of ethanol. The resulting solution was cooled to 10° C. or less with stirring, and 6.0 g (0.12 mol) of hydrazine was added dropwise thereto over 0.5 hours. After the dropwise addition, the solution was stirred at room temperature for 1 hour and subsequently at the reflux temperature for 5 hours. When the reaction was completed, the reaction solution was cooled to room temperature, and 100 mL of water and 20.6 g (0.2 mol) of 35% hydrochloric acid were added thereto. The produced crystal was collected by filtration, washed twice with 10 mL of water and dried by a hot air drier to obtain 12.8 g (yield: 68.1%) of the title compound as a white crystal.

1. temperatureThe resulting solution was cooled to 10° C. or less
2. additionAfter the dropwise addition
3. stirringthe solution was stirred at room temperature for 1 hour and subsequently at the reflux temperature for 5 hours
4. filtrationThe produced crystal was collected by filtration
5. washwashed twice with 10 mL of water
6. customdried by a hot air drier

ORD record

ord-96284dff1c7b460c81f245e200ef5480

Source dataset

uspto-grants-2009_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07488831B2