Ammonia hydroxide → 6-Chloro-2-isopropenyl-3H-quinazolin-4-one

HRID 555258ノート

反応式

HRID 555258 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:11][C:12](=O)[C:13]([CH3:15])=[CH2:14])=[C:6]([CH:10]=1)[C:7]([NH2:9])=[O:8].[OH-].N>CCO>[Cl:1][C:2]1[CH:10]=[C:6]2[C:5](=[CH:4][CH:3]=1)[N:11]=[C:12]([C:13]([CH3:15])=[CH2:14])[NH:9][C:7]2=[O:8]

参加物

4

反応物 2

HCID 21862953Ammonia hydroxideHCID 589496945-Chloro-2-(2-methyl-acryloylamino)-benzamide

生成物 1

HCID 1358145016-Chloro-2-isopropenyl-3H-quinazolin-4-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5-Chloro-2-(2-methyl-acryloylamino)-benzamide (1.5 mmoL) in EtOH (10 mL) was treated with ammonia hydroxide (˜3.0 mmoL) at 80° C. for 4 h. The reaction was then cooled down and the solvent was removed. The reaction mixture was then partitioned between DCM and water. The organic layer was washed with sat. NH4Cl, brine, dried over anhydrous Na2SO4, filtered, concentrated and purified by silica gel column chromatography to afford the title compound as a white solid.

後処理

  1. temperatureThe reaction was then cooled down
  2. customthe solvent was removed
  3. customThe reaction mixture was then partitioned between DCM and water
  4. washThe organic layer was washed with sat. NH4Cl, brine
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-17d31de3cfe84c03a5e1894424813b1b
出典データセット
uspto-grants-2011_11
特許番号
US08053441B2

反応ノート

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