Ethyl isocyanate → HCID 71178974, 화합물

HRID 2409277노트

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HRID 2409277 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]1[N:14]2[N:15]=[CH:16][C:17]([S:18]([NH2:21])(=[O:20])=[O:19])=[C:13]2[N:12]=[CH:11][C:10]=1[C:22]([N:24]1[CH2:29][CH2:28][CH:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:26][CH2:25]1)=[O:23].C(=O)([O-])[O-].[K+].[K+].[CH2:42]([N:44]=[C:45]=[O:46])[CH3:43].[Cl-].[NH4+]>CC(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]1[N:14]2[N:15]=[CH:16][C:17]([S:18]([NH:21][C:45](=[O:46])[NH:44][CH2:42][CH3:43])(=[O:19])=[O:20])=[C:13]2[N:12]=[CH:11][C:10]=1[C:22]([N:24]1[CH2:25][CH2:26][CH:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:28][CH2:29]1)=[O:23]

참가 물질

6

반응물 4

HCID 8022Ethyl isocyanateHCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 71178978HCID 71178978, 화합물

생성물 1

HCID 71178974HCID 71178974, 화합물수율 48%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
50 °C

실험 절차

7-(2-Chlorophenylamino)-6-(4-phenylpiperidine-1-carbonyl)pyrazolo[1,5-a]pyrimidine-3-sulfonamide (0.050 g, 0.098 mmol) obtained in Example 6 step 5 was dissolved in acetone (0.5 mL), potassium carbonate (0.041 g, 0.293 mmol) and ethylisocyanate (0.017 g, 0.245 mmol) were added, and the mixture was stirred at 50° C. for 2 hr. Saturated aqueous ammonium chloride solution was added to quench the reaction, and the mixture was extracted 3 times with ethyl acetate. The organic layers were combined, washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform/methanol=99/1) to give the title compound (0.027 g, 48%).

후처리

  1. customto quench
  2. customthe reaction
  3. extractionthe mixture was extracted 3 times with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography (chloroform/methanol=99/1)

출처 및 근거

ORD 기록
ord-0fe3c72f7af84555aac78b92719e889f
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815874B2

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