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Potassium Carbonate → HCID 44156374、化合物

HRID 1399303
ノート
印刷プレビュー

反応式

HRID 1399303 の反応式
C([O:4][CH:5]([C:8]1[C:13]2[N:14]3[CH2:20][CH2:19][CH2:18][N:17]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=4[Cl:28])[C:15]3=[N:16][C:12]=2[C:11]([Cl:29])=[CH:10][CH:9]=1)[CH2:6][CH3:7])(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:29][C:11]1[C:12]2[N:16]=[C:15]3[N:17]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=4[Cl:28])[CH2:18][CH2:19][CH2:20][N:14]3[C:13]=2[C:8]([CH:5]([OH:4])[CH2:6][CH3:7])=[CH:9][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 441562551-[9-Chloro-1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]propyl acetate

生成物 1

HCID 44156374HCID 44156374、化合物収率 71%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of (+)-1-[9-chloro-1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]propyl acetate (80.6 mg, 0.178 mmol) in methanol (1.5 mL) was added potassium carbonate (36.9 mg, 0.267 mmol). The reaction mixture was stirred at room temperature for 1.5 hrs. After the mixture was concentrated, the residue was diluted with water and extracted with ethyl acetate (×3). The combined organic layer was washed with brine (×1), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 0-50% ethyl acetate/n-hexane gradient mixture. The resulting solid was recrystallized from ethyl acetate/n-hexane to give the title compound as a colorless powder (51.6 mg, 0.126 mmol, 71%).

後処理

  1. concentrationAfter the mixture was concentrated
  2. additionthe residue was diluted with water
  3. extractionextracted with ethyl acetate (×3)
  4. washThe combined organic layer was washed with brine (×1)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by silica gel column chromatography
  9. washeluting with a 0-50% ethyl acetate/n-hexane gradient mixture
  10. customThe resulting solid was recrystallized from ethyl acetate/n-hexane

出典と根拠

ORDレコード
ord-b4442db2755c4a92a7a3a5e35d701940
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08901141B2

反応ノート

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