Potassium Carbonate → HCID 58853204, 화합물

HRID 2280876노트

반응식

HRID 2280876 반응식
F[C:2](F)(F)[C:3]1[CH:8]=[CH:7][C:6]([CH:9]([NH2:13])[CH2:10][CH2:11][CH3:12])=[CH:5][CH:4]=1.[Cl:16][C:17]1[CH:22]=[N:21][CH:20]=[C:19](Cl)[N:18]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C(OCC)(=O)C.O>[Cl:16][C:17]1[N:18]=[C:19]([NH:13][CH:9]([C:6]2[CH:7]=[CH:8][C:3]([CH3:2])=[CH:4][CH:5]=2)[CH2:10][CH2:11][CH3:12])[CH:20]=[N:21][CH:22]=1

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 785042,6-DichloropyrazineHCID 59339521HCID 59339521, 화합물

생성물 1

HCID 58853204HCID 58853204, 화합물수율 5.7%

시약·촉매·용매 3

HCID 962Water용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of 1-[4-(trifluoromethyl)phenyl]butan-1-amine (0.40 g, 1.9 mmol) and 2,6-dichloropyrazine (0.55 g, 3.7 mmol) in 1,4-dioxane (6 mL) was added anhydrous potassium carbonate (0.39 g, 2.8 mmol). The resulting mixture was heated at reflux for 18 h. After cooling to room temperature, the mixture was diluted with ethyl acetate and H2O. The organic phase was collected, dried and concentrated. The residue was purified by flash chromatography eluting with ethyl acetate-hexane (1:1) to give pure product (0.03 g, 5%).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 18 h
  3. customThe organic phase was collected
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by flash chromatography
  7. washeluting with ethyl acetate-hexane (1:1)

출처 및 근거

ORD 기록
ord-1f15f0a932a64a9caa52d8e11c824d3d
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09139560B2

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