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Dimethylamine → HCID 23369747、化合物

HRID 1900791
ノート
印刷プレビュー

反応式

HRID 1900791 の反応式
[OH:1][C:2]1[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6](=[O:13])[NH:7]2.[CH3:14][NH:15][CH3:16].[CH2:17]=O>CN(C)C=O>[CH3:14][N:15]([CH2:17][C:11]1[C:2]([OH:1])=[C:3]2[C:8](=[C:9]([CH3:12])[CH:10]=1)[NH:7][C:6](=[O:13])[CH:5]=[CH:4]2)[CH3:16]
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 674Dimethylamine2 回HCID 712Formaldehyde2 回HCID 23369598HCID 23369598、化合物

生成物 1

HCID 23369747HCID 23369747、化合物収率 94.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

5-Hydroxy-8-methylcarbostyril (10.51 g, 60 mmol) and dimethylamine (aqueous 40% solution, 12.07 g, 66 mmol) were dissolved in N,N-dimethylformamide (30 ml). To this solution, formaldehyde (aqueous 37% solution, 5.36 g, 66 mmol) was added slowly at room temperature, and stirred. After 12 hours, dimethylamine (6 g, 33 mmol), formaldehyde (2.79 g, 33 mmol), and N,N-dimethylformamide (20 ml) were added thereto, and the mixture was stirred at room temperature for further 12 hours. After completion of the reaction, the solvent was distilled off under reduced pressure, and the resultant residue was combined with chloroform and n-hexane. Crystals were collected by filtration, and dried under reduced pressure. As a result, 13.23 g of the title compound was obtained as pale reddish gray crystals (95%).

後処理

  1. stirringthe mixture was stirred at room temperature for further 12 hours
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. filtrationCrystals were collected by filtration
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-c7ec74a4c0de4bb29f0e34d12f2853fe
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05576324

反応ノート

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