1,4-Dioxane hydrochloride → 1-(2-toluoylmethyl)-2-oxo-3-amino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine

HRID 1979296ノート

反応式

HRID 1979296 の反応式
Cl.O1CCOCC1.[C:8]1([CH3:43])[C:9]([C:14]([CH2:16][N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[N:21]([C:28](=[O:33])[C:29]([CH3:32])([CH3:31])[CH3:30])[CH2:20][CH:19]([NH:34]C(OC(C)(C)C)=O)[C:18]2=[O:42])=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=1>C(O)C>[C:8]1([CH3:43])[C:9]([C:14]([CH2:16][N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[N:21]([C:28](=[O:33])[C:29]([CH3:31])([CH3:32])[CH3:30])[CH2:20][CH:19]([NH2:34])[C:18]2=[O:42])=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 21201777HCID 21201777、化合物

生成物 1

HCID 212016481-(2-toluoylmethyl)-2-oxo-3-amino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine収率 95.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

4N HCl-dioxane solution (5 ml) was added to 1-(2-toluoylmethyl)-2-oxo-3-tert-butoxycarbonylamino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (540 mg) in ethanol (5 ml), and the mixture was stirred at 50° C. for 30 minutes. The reaction mixture was concentrated under reduced pressure, and saturated aqueous sodium bicarbonate solution was added to the residue, followed by extraction with methylene chloride. The extract was dried over anhydrous sodium sulfate, to thereby obtain 411 mg of the titled compound.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and saturated aqueous sodium bicarbonate solution
  2. additionwas added to the residue
  3. extractionfollowed by extraction with methylene chloride
  4. dry with materialThe extract was dried over anhydrous sodium sulfate

出典と根拠

ORDレコード
ord-34640dd01b5e4768b190d6a6e5e895f9
出典データセット
uspto-grants-2001_05
特許番号
US06239131B1

反応ノート

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