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HCID 47174299, 화합물 → HCID 178448624, 화합물

HRID 2042718
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HRID 2042718 반응식
[CH2:1]([NH:5][C:6]1[CH:11]=[N:10][N:9]([CH3:12])[C:8](=[O:13])[C:7]=1Cl)[CH2:2][CH2:3][CH3:4].[F:15][C:16]1[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][C:17]=1[C:18]([N:20]=[C:21]=[S:22])=[O:19]>O1CCOCC1>[CH2:1]([N:5]1[C:6]2[CH:11]=[N:10][N:9]([CH3:12])[C:8](=[O:13])[C:7]=2[S:22]/[C:21]/1=[N:20]\[C:18](=[O:19])[C:17]1[CH:23]=[C:24]([C:27]([F:30])([F:29])[F:28])[CH:25]=[CH:26][C:16]=1[F:15])[CH2:2][CH2:3][CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 47174299HCID 47174299, 화합물HCID 54578953HCID 54578953, 화합물

생성물 1

HCID 178448624HCID 178448624, 화합물수율 22.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A mixture of 5-(butylamino)-4-chloro-2-methylpyridazin-3(2H)-one from Example 4A (250 mg, 1.16 mmol) and 2-fluoro-5-(trifluoromethyl)benzoyl isothiocyanate (375 mg, 1.51 mmol) in dioxane (20 mL) was heated at 70° C. for 12 hours and at 100° C. for 6 hours. The mixture was concentrated under reduced pressure and the residue was dissolved in EtOAc, washed with saturated aqueous NaHCO3 and brine, dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by chromatography (CH2Cl2-Et2O 19:1)) to afford 110 mg of the title compound. MS (ESI) m/z 429 (M+H)+.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in EtOAc
  3. washwashed with saturated aqueous NaHCO3 and brine
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by chromatography (CH2Cl2-Et2O 19:1))

출처 및 근거

ORD 기록
ord-eb446848884d40ffa48b0f2f1a164784
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586596B2

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