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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Carbon Tetrachloride → HCID 66607261, 화합물

HRID 71105
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HRID 71105 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([NH:12][NH:13][C:14](=O)[C:15]2[CH:20]=[CH:19][C:18]([C:21]3[O:25][C:24]([CH3:26])=[N:23][CH:22]=3)=[C:17]([O:27][CH3:28])[CH:16]=2)=[O:11])[CH:5]=[CH:6][C:7]=1[F:8].C(Cl)(Cl)(Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(#N)C>[F:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][C:7]=1[F:8])[CH2:9][C:10]1[O:11][C:14]([C:15]2[CH:20]=[CH:19][C:18]([C:21]3[O:25][C:24]([CH3:26])=[N:23][CH:22]=3)=[C:17]([O:27][CH3:28])[CH:16]=2)=[N:13][N:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 66607891N'-[(3,4-difluorophenyl)acetyl]-3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)benzohydrazide

생성물 1

HCID 66607261HCID 66607261, 화합물수율 53.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
80 °C

실험 절차

A mixture of N′-[(3,4-difluorophenyl)acetyl]-3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)benzohydrazide (4.69 g), carbon tetrachloride (2.24 mL) and triphenylphosphine (12.3 g) in acetonitrile (117 mL) was stirred at 80° C. for 2 hr. The mixture was allowed to cool to room temperature, the precipitate was filtered off, and the filtrate was concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate). Ethyl acetate was added to the obtained crude product, the precipitate was filtered off, and the filtrate was concentrated. Acetonitrile was added to the obtained residue, and the resultant precipitate was collected by filtration to give the title compound (2.41 g).

후처리

  1. temperatureto cool to room temperature
  2. filtrationthe precipitate was filtered off
  3. concentrationthe filtrate was concentrated
  4. additionWater was added to the residue
  5. extractionthe mixture was extracted with ethyl acetate
  6. dry with materialThe extract was dried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (ethyl acetate)
  9. additionEthyl acetate was added to the
  10. customobtained crude product
  11. filtrationthe precipitate was filtered off
  12. concentrationthe filtrate was concentrated
  13. additionAcetonitrile was added to the obtained residue
  14. filtrationthe resultant precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-79c8850a2800400a9fb5762436a9d847
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822699B2

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