ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Chloroacetyl chloride → 5-methyl-1H-pyrido[2,3-b][1,4]oxazin-2-one

HRID 1943746
ノート
印刷プレビュー

反応式

HRID 1943746 の反応式
[NH2:1][C:2]1[C:3]([OH:9])=[N:4][CH:5]=[C:6](C)[CH:7]=1.Cl[CH2:11][C:12](Cl)=[O:13].[C:15](=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:15][N:4]1[CH:3]2[O:9][CH2:11][C:12](=[O:13])[NH:1][C:2]2=[CH:7][CH:6]=[CH:5]1
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 6577Chloroacetyl chlorideHCID 11430Potassium CarbonateHCID 178430713HCID 178430713、化合物

生成物 1

HCID 669367555-methyl-1H-pyrido[2,3-b][1,4]oxazin-2-one収率 24.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3-amino-5-methyl-pyridin-2-ol (1.32 g, 10.6 mmol) was dissolved in 50 ml of anhydrous N,N-dimethyl formamide under nitrogen atmosphere, and chloroacetyl chloride solution (1.02 ml, 12.72 mmol) was added thereto dropwise at room temperature. After stirring for 30 minutes, potassium carbonate (3.7 g, 26.5 mmol) was added thereto dropwise at room temperature, and the reaction mixture was heated to 100□ and then stirred for 18 hours. The reaction mixture was cooled to room temperature and the reaction was quenched by adding water. The organic layer was extracted with ethyl acetate, and the combined organic layer was washed with water and saturated saline solution, dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain straw yellow solid (424 mg). The resulting solid was used in the next step without further purification.

後処理

  1. customdropwise at room temperature
  2. stirringstirred for 18 hours
  3. temperatureThe reaction mixture was cooled to room temperature
  4. customthe reaction was quenched
  5. additionby adding water
  6. extractionThe organic layer was extracted with ethyl acetate
  7. washthe combined organic layer was washed with water and saturated saline solution
  8. dry with materialdried over anhydrous sodium sulfate (Na2SO4)
  9. filtrationfiltered
  10. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-07ce11b96d2c4160bfc8bc5afd657df0
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08394792B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート