Potassium Carbonate → 1-[5-(4-Chlorophenyl)-6-(2,4-dichlorophenyl)-3-(methylamino)furo-[2,3-b]pyridin-2-yl]-2,2-dimethylpropan-1-one

HRID 8793노트

반응식

HRID 8793 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[C:10]3[C:24]([N:25](C)[C:26](=O)C(F)(F)F)=[C:23]([C:33](=[O:38])[C:34]([CH3:37])([CH3:36])[CH3:35])[O:22][C:11]3=[N:12][C:13]=2[C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=2[Cl:21])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+]>CO.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[C:10]3[C:24]([NH:25][CH3:26])=[C:23]([C:33](=[O:38])[C:34]([CH3:36])([CH3:35])[CH3:37])[O:22][C:11]3=[N:12][C:13]=2[C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=2[Cl:21])=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 21984837N-[5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)-2-(2,2-dimethylpropanoyl)furo[2,3-b]pyridin-3-yl]-2,2,2-trifluoro-N-methylacetamide

생성물 1

HCID 100969791-[5-(4-Chlorophenyl)-6-(2,4-dichlorophenyl)-3-(methylamino)furo-[2,3-b]pyridin-2-yl]-2,2-dimethylpropan-1-one

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A solution of the product from Step A (0.0703 mmol) in methanol (2 mL) and water (0.1 mL) was treated with potassium carbonate (0.049 g; 0.351 mmol) at room temperature. The reaction mixture was stirred a room temperature until the reaction was judged complete by TLC analysis. The reaction mixture was then partitioned between ethyl acetate and saturated NaHCO3 solution. The organic layer was washed twice with saturated NaHCO3 solution, brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by MPLC (silica gel; 0% to 20% ethyl acetate:hexane gradient) gave the title compound. HPLC/MS: 487.0 (M+1), 489.0 (M+3); Rt=5.03 min.

후처리

  1. customThe reaction mixture was then partitioned between ethyl acetate and saturated NaHCO3 solution
  2. washThe organic layer was washed twice with saturated NaHCO3 solution, brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customPurification by MPLC (silica gel; 0% to 20% ethyl acetate:hexane gradient)

출처 및 근거

ORD 기록
ord-679402d1219b469b81cbcf32fa23699d
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091216B2

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