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Potassium Carbonate → HCID 23053773, 화합물

HRID 1650152
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HRID 1650152 반응식
P(Cl)(Cl)(Cl)=O.[CH3:6][C:7]1[CH:15]=[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][N:9]2[N:8]=1.[C:16](=O)([O-])[O-:17].[K+].[K+]>CN(C)C=O>[CH:16]([C:15]1[C:7]([CH3:6])=[N:8][N:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=12)=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 24813Phosphorus oxychlorideHCID 15620341HCID 15620341, 화합물

생성물 1

HCID 23053773HCID 23053773, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 116.6 ml of dimethylformamide was added 105 ml of phosphorus oxychloride, followed by 99 g of 2-methylpyrazolo[1,5-a]pyridine under stirring at keeping the temperature below 20° C. The reaction mixture was stirred at 50°-60° C. for 1 hours, then poured into ice water. Acidic aqueous solution was neutralized with potassium carbonate, then extracted with dichloromethane, washed with salt water, dried over anhydrous sodium sulfate and then concentrated. The resulting residue was recrystallized from methanol to give the title compound in a yield of 54.8 g (46%) as colorless crystals, mp 77°-79° C.

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후처리

  1. customthe temperature below 20° C
  2. stirringThe reaction mixture was stirred at 50°-60° C. for 1 hours
  3. extractionextracted with dichloromethane
  4. washwashed with salt water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe resulting residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-96030ff1648e481399bba50cc3765f2a
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04923871

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