Hydrochloric Acid → HCID 178516151, 화합물

HRID 1172092

반응식

HRID 1172092 반응식
[C:1]1([NH:7][NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[F:10][C:11]([F:21])([F:20])[C:12](=O)[CH2:13][C:14](OCC)=[O:15]>C(O)C>[C:1]1([N:7]2[C:14]([OH:15])=[CH:13][C:12]([C:11]([F:21])([F:20])[F:10])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7516PhenylhydrazineHCID 67793Ethyl 4,4,4-trifluoroacetoacetate

생성물 1

HCID 178516151HCID 178516151, 화합물수율 87.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

20 g (184.9 mmoles) of phenylhydrazine and 4 ml of concentrated hydrochloric acid were added to a solution of 34.1 g (184.9 mmoles) of ethyl trifluoroacetoacetate dissolved in 500 ml of ethanol. The mixture was refluxed for 1 hour with heating, to give rise to a reaction. After the completion of the reaction, the reaction mixture was subjected to vacuum distillation to remove the most part of the solvent contained therein. The residue was mixed with water to precipitate crystals. The crystals were collected by filtration, washed with water until the filtrate became neutral, and dried to obtain 37.1 g (yield: 87.9%) of 1-phenyl-3-trifluoromethyl-1H-pyrazol-5-ol as ocherous crystals.

후처리

  1. temperatureThe mixture was refluxed for 1 hour
  2. temperaturewith heating
  3. customto give rise
  4. customto a reaction
  5. customAfter the completion of the reaction
  6. distillationthe reaction mixture was subjected to vacuum distillation
  7. customto remove the most part of the solvent
  8. additionThe residue was mixed with water
  9. customto precipitate crystals
  10. filtrationThe crystals were collected by filtration
  11. washwashed with water until the filtrate
  12. customdried

출처 및 근거

ORD 기록
ord-9a60088a76c1448b84b60816149a115f
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07833939B2

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