Potassium Carbonate → HCID 67055245, 화합물

HRID 601655

반응식

HRID 601655 반응식
[CH3:1][NH:2][CH:3]([CH3:5])[CH3:4].C(=O)([O-])[O-].[K+].[K+].CN(C)S(=O)=O.Cl[C:19]1[CH:28]=[CH:27][C:26]2[C:21](=[CH:22][CH:23]=[C:24]([Br:29])[CH:25]=2)[N:20]=1>O>[Br:29][C:24]1[CH:25]=[C:26]2[C:21](=[CH:22][CH:23]=1)[N:20]=[C:19]([N:2]([CH3:1])[CH:3]([CH3:5])[CH3:4])[CH:28]=[CH:27]2

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 78485N-MethylisopropylamineHCID 128940866-Bromo-2-chloroquinolineHCID 178486088HCID 178486088, 화합물

생성물 1

HCID 67055245HCID 67055245, 화합물수율 2.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

Under nitrogen atmosphere, 180 mg of N-methylisopropylamine, and 200 g of potassium carbonate were added at room temperature sequentially to 5 ml solution of dimethylsulfonamide with 63 g of 2-chloro-6-bromoquinoline, and the mixture was stirred at 110° C. for 4 hours. Water was added to the reaction solution, extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution, and dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure, and the residues were separated and purified by silicagel chromatography (hexane/ethyl acetate=3/1) to obtain 18 mg of the above compound as a white solid.

후처리

  1. extractionextracted with ethyl acetate
  2. washEthyl acetate layer was washed with saturated saline solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationThe solvents were distilled outunder reduced pressure
  5. customthe residues were separated
  6. custompurified by silicagel chromatography (hexane/ethyl acetate=3/1)

출처 및 근거

ORD 기록
ord-1c89321693754e3bb4331fa3b6b35c4c
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902369B2

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