Acetic Acid → HCID 178516151, 화합물

HRID 1159480

반응식

HRID 1159480 반응식
[F:1][C:2]([F:12])([F:11])[C:3](=O)[CH2:4][C:5]([O:7]CC)=O.C(O)(=O)C.[C:17]1([NH:23][NH2:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[OH:7][C:5]1[N:23]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:24]=[C:3]([C:2]([F:1])([F:11])[F:12])[CH:4]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 7516PhenylhydrazineHCID 67793Ethyl 4,4,4-trifluoroacetoacetate

생성물 1

HCID 178516151HCID 178516151, 화합물수율 98%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
10 °C

실험 절차

18.4 g (0.1 mole) of ethyl 4,4,4-trifluoroacetoacetate was dissolved in 12.0 g (0.2 mole) of acetic acid. The solution was cooled to 10° C. or lower with stirring. Thereto was dropwise added, in 0.5 hour, 11.8 g (0.11 mole) of phenylhydrazine. 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 100 ml of water. The resulting crystals were collected by filtration, washed with 50 ml of water twice, and dried in a hot-air drier, to obtain 22.3 g (yield: 98.0%) of a title compound as light yellow crystals.

후처리

  1. additionThereto was dropwise added, in 0.5 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. filtrationThe resulting crystals were collected by filtration
  9. washwashed with 50 ml of water twice
  10. customdried in a hot-air drier,

출처 및 근거

ORD 기록
ord-ccef4bbee4aa4a869de99b8b2947ce1a
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812175B2

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