Methane → HCID 178516151, 화합물

HRID 1289867

반응식

HRID 1289867 반응식
[F:1][C:2]([F:12])([F:11])[C:3](=O)[CH2:4][C:5]([O:7]CC)=O.[C:13]1([NH:19][NH2:20])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.Cl.C>CO>[C:13]1([N:19]2[C:5]([OH:7])=[CH:4][C:3]([C:2]([F:1])([F:11])[F:12])=[N:20]2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

6

반응물 4

HCID 297MethaneHCID 313Hydrochloric AcidHCID 7516PhenylhydrazineHCID 67793Ethyl 4,4,4-trifluoroacetoacetate

생성물 1

HCID 178516151HCID 178516151, 화합물수율 79.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 44 ml (0.3 mol) of ethyl trifluoroacetoacetate and 33 mL (335.4 mmol) of phenylhydrazine in 60 ml of methanol containing 6 ml of conc. HCl solution was refluxed with stirring for 1.5 hours. After adding activated charcoal with stirring, the hot mixture was filtered. The residue was washed with methanol (2×70 ml), diluted with water, and the resulting white solid was filtered. The solid was washed with hexane and dried to afford 54.3 g (79%) of 1-phenyl-3-trifluoromethyl-5-hydroxypyrazole as a pale solid.

후처리

  1. temperaturewas refluxed
  2. stirringwith stirring
  3. filtrationthe hot mixture was filtered
  4. washThe residue was washed with methanol (2×70 ml)
  5. additiondiluted with water
  6. filtrationthe resulting white solid was filtered
  7. washThe solid was washed with hexane
  8. customdried

출처 및 근거

ORD 기록
ord-98dfa323a2214946b4c50a2aed386206
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750550

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