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Chloroform → 2-(4-Dimethylamino-butyl)-5,6-dimethoxy-1-methyl-1H-quinazoline-4-one

HRID 557150
ノート
印刷プレビュー

反応式

HRID 557150 の反応式
[CH3:1][N:2]([CH:4]([CH2:8][CH2:9][CH3:10])C(O)=O)[CH3:3].S(Cl)(Cl)=O.[CH3:15][NH:16][C:17]1[C:22]([C:23]([NH2:25])=[O:24])=[C:21]([O:26][CH3:27])[C:20]([O:28][CH3:29])=[CH:19][CH:18]=1.Cl[CH:31](Cl)Cl>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:8][CH2:9][CH2:10][C:15]1[N:16]([CH3:31])[C:17]2[C:22]([C:23](=[O:24])[N:25]=1)=[C:21]([O:26][CH3:27])[C:20]([O:28][CH3:29])=[CH:19][CH:18]=2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 6212ChloroformHCID 24386Thionyl ChlorideHCID 178834622-(Dimethylamino)pentanoic acidHCID 669909586-Methylamino-2,3-dimethoxybenzamide

生成物 1

HCID 669913772-(4-Dimethylamino-butyl)-5,6-dimethoxy-1-methyl-1H-quinazoline-4-one

反応条件

温度
57.5 °C

実験手順

3.80 g (20.9 mmol) Dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (11.1 mmol) 6-methylamino-2,3-dimethoxybenzamide dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 2 h and stirred overnight at room temperature. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum.

後処理

  1. distillationThe remaining thionyl chloride was distilled in vacuum
  2. waitThe mixture was boiled for 2 h
  3. stirringstirred overnight at room temperature
  4. filtrationAfter filtration the residue
  5. dissolutionwas dissolved in trichloromethane
  6. dry with materialThe organic solution was dried over magnesium sulfate
  7. customevaporated under vacuum

出典と根拠

ORDレコード
ord-1a77a7c056f24f0d8f7fce86aedb7dfd
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058431B2

反応ノート

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