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Water → (3s)-3-Methyl-2,3,4,5-tetrahydro-1h-1,4-benzodiazepin-9-amine

HRID 1082055
ノート
印刷プレビュー

反応式

HRID 1082055 の反応式
[NH2:1][C:2]1[C:12]2[NH:11][C:10](=O)[C@H:9]([CH3:14])[NH:8][C:7](=O)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCOCC1>[CH3:14][C@@H:9]1[NH:8][CH2:7][C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([NH2:1])[C:12]=2[NH:11][CH2:10]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 962Water2 回HCID 14798Sodium HydroxideHCID 11095747HCID 11095747、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 11829983(3s)-3-Methyl-2,3,4,5-tetrahydro-1h-1,4-benzodiazepin-9-amine収率 99.5%

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

実験手順

14.8 g (0.072 mol) of (S)-9-amino-3-methyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione in 455 ml of dioxane are heated at the reflux temperature with stirring for 48 hours in the presence of 17 g of lithium aluminium hydride. The reaction mixture is cooled in an ice bath and then, slowly and successively, 17 ml of water, 17 ml of a 5N sodium hydroxide solution and 45 ml of water are added. The mixture is left stirring for 2 hours at room temperature, filtration is carried out and washing is carried out with hot tetrahydrofuran and with dichloromethane. The organic phase is recovered and is concentrated. There are obtained 12.7 g of product which is used as is in the following stage.

後処理

  1. temperatureThe reaction mixture is cooled in an ice bath
  2. waitThe mixture is left
  3. filtrationfiltration
  4. washwashing
  5. customThe organic phase is recovered
  6. concentrationis concentrated

出典と根拠

ORDレコード
ord-f85504502baf461f9da5886cb89b7173
出典データセット
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05589476

反応ノート

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