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Dimethylformamide → 2,11-dihydro-2-methyl-3H-s-triazolo[3,4-b][3]benzazepin-3-one

HRID 1414722
ノート
印刷プレビュー

反応式

HRID 1414722 の反応式
[N:1]1[NH:2][C:3](=[O:15])[N:4]2[CH:10]=[CH:9][C:8]3[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=3[CH2:6][C:5]=12.[CH3:16]N(C)C=O.[OH-].[Na+].CI>O>[CH3:16][N:2]1[C:3](=[O:15])[N:4]2[C:5]([CH2:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[CH:10]2)=[N:1]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 130667602,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

生成物 1

HCID 130667612,11-dihydro-2-methyl-3H-s-triazolo[3,4-b][3]benzazepin-3-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 8 parts of 2,11-dihydro-3H-s-triazolo-[3,4-b][3]benzazepin-3-one in 80 volume parts of dimethylformamide is added 9 volume parts of 5N aqueous sodium hydroxide solution and then 3 volume parts of methyl iodide is added dropwise under stirring. After stirring for 1 hour, the reaction mixture is diluted with water and extracted with ethyl acetate. The ethyl acetate layer is washed with water and the solvent is distilled off. The precipitate is collected by filtration to give 2,11-dihydro-2-methyl-3H-s-triazolo[3,4-b][3]benzazepin-3-one as crystals. Recrystallization from isopropyl ether gives light-brown needles melting at 123° -124° C.

後処理

  1. stirringAfter stirring for 1 hour
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer is washed with water
  4. distillationthe solvent is distilled off
  5. filtrationThe precipitate is collected by filtration

出典と根拠

ORDレコード
ord-d48b59df7efa49cf8c9a8645b6cea471
出典データセット
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04002638

反応ノート

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