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 8793ノート

反応式

HRID 8793 の反応式
[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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-679402d1219b469b81cbcf32fa23699d
出典データセット
uspto-grants-2006_08
特許番号
US07091216B2

反応ノート

読み込み中…