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Potassium Carbonate → HCID 58960243、化合物

HRID 2068119
ノート
印刷プレビュー

反応式

HRID 2068119 の反応式
[F:1][C:2]1[C:10]([O:11][C:12]2[C:21]3[C:16](=[CH:17][C:18]([OH:24])=[C:19]([O:22][CH3:23])[CH:20]=3)[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:25])[NH:6]2.S(C1C=CC(C)=CC=1)(O[CH2:30][CH:31]1[O:33][CH2:32]1)(=O)=O.C(=O)([O-])[O-].[K+].[K+]>CC(N(C)C)=O>[F:1][C:2]1[C:10]([O:11][C:12]2[C:21]3[C:16](=[CH:17][C:18]([O:24][CH2:30][C@H:31]4[CH2:32][O:33]4)=[C:19]([O:22][CH3:23])[CH:20]=3)[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:25])[NH:6]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 160868Glycidyl tosylateHCID 1355308324-((4-Fluoro-2-methyl-1H-indol-5-yl)oxy)-6-methoxyquinazolin-7-ol

生成物 1

HCID 58960243HCID 58960243、化合物収率 85.7%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

4-(4-Fluoro-2-methylindol-5-yloxy)-7-hydroxy-6-methoxyquinazoline (339 mg, 1 mmol), (prepared as described for the starting material in Example 7), was dissolved in dimethylacetamide (5 ml) under nitrogen. (2R) Glycidyl tosylate (285 mg, 1.25 mmol) and potassium carbonate (345 mg, 2.5 mmol) were added and the reaction stirred at ambient temperature for 2.5 hours, then warmed to 40° C. and left overnight. The solvent was removed under vacuum and the residue partitioned between water and dichloromethane. The organic phase was washed with brine and dried (Na2SO4). The residue was purified by column chromatography, eluting with methylene chloride/methanol (97/3) to give 4-[(4-Fluoro-2-methyl-1H-indol-5-yl)oxy]-6-methoxy-7-[(2R)-oxiran-2-ylmethoxy]quinazoline (339 mg, 85%).

後処理

  1. temperaturewarmed to 40° C.
  2. waitleft overnight
  3. customThe solvent was removed under vacuum
  4. customthe residue partitioned between water and dichloromethane
  5. washThe organic phase was washed with brine
  6. dry with materialdried (Na2SO4)
  7. customThe residue was purified by column chromatography
  8. washeluting with methylene chloride/methanol (97/3)

出典と根拠

ORDレコード
ord-67e455b1996a45479f97e1787e893bbe
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08293902B2

反応ノート

読み込み中…

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